WO2020029019A1 - Nouvelle silice précipitée et son procédé de préparation - Google Patents

Nouvelle silice précipitée et son procédé de préparation Download PDF

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Publication number
WO2020029019A1
WO2020029019A1 PCT/CN2018/098994 CN2018098994W WO2020029019A1 WO 2020029019 A1 WO2020029019 A1 WO 2020029019A1 CN 2018098994 W CN2018098994 W CN 2018098994W WO 2020029019 A1 WO2020029019 A1 WO 2020029019A1
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Prior art keywords
units
och
substance
unit
white carbon
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PCT/CN2018/098994
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English (en)
Chinese (zh)
Inventor
陈树真
李锐
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湖州五爻硅基材料研究院有限公司
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Priority to CN201880090624.3A priority Critical patent/CN111867974B/zh
Priority to PCT/CN2018/098994 priority patent/WO2020029019A1/fr
Publication of WO2020029019A1 publication Critical patent/WO2020029019A1/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

Definitions

  • the present invention relates to silica, and more particularly, to a novel precipitated white carbon black and a preparation method thereof.
  • Precipitated silica is also called hydrated silica, activated silica, precipitated silica, and precipitated hydrated silica. Its chemical structure is the Q unit of Si, namely SiO 4- . It is mainly used for natural rubber and synthetic rubber. Reinforcing agents, matting agents for coatings, etc. The existing precipitated white carbon powder has serious agglomeration, which brings great inconvenience to its dispersion in rubber, coatings, etc., and limits its function.
  • CN201310374881.9, US9688784B2, US8846806B2 each disclose a method for improving the dispersion of precipitated white carbon black. These dispersion methods all improve the dispersibility by adding polymer surfactants, and obviously do not solve the dispersion problem at all.
  • the present invention aims to provide a novel precipitated white carbon black and a preparation method thereof.
  • the specific surface area of the new precipitated white carbon black is greater than 100 m 2 / g.
  • the specific surface area is between 150m 2 / g-270m 2 / g.
  • the invention also provides a method for preparing a new type of precipitated white carbon black, in which a substance that generates Q units and a substance that generates D units are subjected to a water condensation reaction under an environment of pH 8-11 to form a condensate, and the condensate is washed and dried A new type of precipitated white carbon black is obtained, and the weight ratio of D units to Q units in the new type of precipitated white carbon is between 0.05 and 0.19; wherein the substance that generates Q units is selected from at least one of the group consisting of One type: water glass, tetraethoxysilane, tetramethoxysilane, tetrachlorosilane; wherein the substance generating D units is at least one selected from the group consisting of: (CH 3 ) 2 Si (OCH 3 ) 2 , (CH 3 ) 2 Si (OCH 2 CH 3 ) 2 , (CH 3 ) HSi (OCH 3 ) 2 , (CH 3 )
  • the condensate is washed with filter press water, and the filter cake is heated and dried in an electric furnace to be dispersed into a finished product.
  • the filter cake can also be spray-dried and dispersed into a finished product after repulping.
  • the preparation method includes adding a silane coupling agent for processing to improve the affinity with the organic polymer.
  • the silane coupling agent may be added at the same time as the substance that generates D units, or may be added after the condensation product is formed, or it may be added after the condensation product is washed.
  • the silane coupling agent is at least one selected from the group consisting of the following coupling agents: vinyltrichlorosilane, vinyltrimethoxysilane, vinyltriethoxysilane, 2- (3,4 Epoxycyclohexyl) ethyltrimethoxysilane, (3-glycidoxypropyl) trimethoxysilane, (3-glycidoxypropyl) methyldiethoxysilane, (3- Glycidoxypropyl) triethoxysilane, p-styryltrimethoxysilane, 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyl Methyldiethoxysilane, 3-methacryloyloxypropyltriethoxysilane, 3-acryloyloxypropyltrimethoxysilane, N-2aminoethyl-3-aminopropylmethyldi Methoxysilane, N-2aminoe
  • the preparation method includes the steps of: S1, providing an aqueous solution of a substance that generates Q units; and S2, adding a substance that generates D units to the aqueous solution to perform a water condensation reaction.
  • S1 providing an aqueous solution of a substance that generates Q units
  • S2 adding a substance that generates D units to the aqueous solution to perform a water condensation reaction.
  • the substance that generates D units can also be added to the solvent to form an aqueous solution at the same time as the substance that generates Q units to perform a water condensation reaction.
  • the aqueous solution is an aqueous solution of water glass with a silica mass fraction of 2-10%.
  • the water glass is diluted with deionized water to a silica mass fraction of 2-10% in order to control the reaction.
  • water glass having a silica mass fraction of 30% was diluted with deionized water to an aqueous solution having a silica mass fraction of 5%.
  • the aqueous solution is an alcohol-water mixed solution of tetraethoxysilane (or tetrachlorosilane), such as an isopropanol aqueous solution.
  • tetraethoxysilane or tetrachlorosilane
  • isopropanol aqueous solution 173.6 g of tetraethoxysilane (or 142 g of tetrachlorosilane) was dissolved in 800 g of a 50% by weight aqueous solution of isopropanol.
  • step S2 the water-containing condensation reaction is performed in a range of room temperature to 100 degrees.
  • the water-containing condensation reaction is heated to 50-70 degrees, preferably 60 degrees, under stirring conditions.
  • the hydrocondensation reaction is performed in a reaction vessel with a heater and a stirrer.
  • step S2 the pH is adjusted to 8-11 directly to perform the water condensation reaction before adding the substance that generates D units.
  • the pH of the D-unit-generating substance is adjusted to be acidic before the D-unit-generating substance is added to facilitate the dissolution of the D-unit-generating substance in an aqueous solution, and then the pH is adjusted to 8-11 to perform the water condensation reaction.
  • a substance that generates D units is added, and then adjusted to 9 to perform a water condensation reaction.
  • the pH is adjusted by the dropwise addition of sulfuric acid (or ammonia or an inorganic base such as an aqueous solution of sodium hydroxide), preferably sulfuric acid (or ammonia or an aqueous solution of sodium hydroxide) at a concentration of 5% (mass fraction) is added dropwise Adjust the pH.
  • sulfuric acid or ammonia or an inorganic base such as an aqueous solution of sodium hydroxide
  • sulfuric acid or ammonia or an aqueous solution of sodium hydroxide
  • the novel precipitated white carbon of the present invention introduces D units on the basis of Q units, that is, R 1 R 2 SiO 2- (R 1 and R 2 are Hydrocarbon or hydrogen can be independently selected), and the weight ratio of D units to Q units is controlled between 0.05-0.19 in a targeted manner, which can solve the dispersion problem of precipitated white carbon black.
  • the specific surface area of the novel precipitated white carbon black according to the present invention is greater than 100 m 2 / g, which can maintain the filler effect such as the reinforcement of the precipitated white carbon black.
  • Judging the difficulty of the dispersion of the powder obtained in the following examples includes the method of placing the powder in methyl ethyl ketone and measuring the intensity distribution by irradiating with 500W ultrasonic waves for 3 minutes.
  • D 90 is less than 20 microns for easy dispersion, and D 90 is greater than 50 microns for difficult dispersion.
  • the Q unit and D unit content in the powders obtained in the following examples can be determined from the chemical integral of the solid 29 SiNMR spectrum in the range of -80 to -120 ppm. The integrated area of the front within the 30 ppm range (proportional to the D unit content) was calculated.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees under stirring conditions, and the pH was adjusted to 8 by adding 5% sulfuric acid dropwise. 7 g of dimethyldimethoxysilane was added and reacted at 60 degrees for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain the powder of Example 1.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.086.
  • the powder was put into methyl ethyl ketone, and the intensity distribution was measured after irradiating with 500 W ultrasonic waves for 3 minutes. It was found that D 90 was 12 ⁇ m.
  • the specific surface area measured by the nitrogen adsorption method was 190 m 2 / g.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees under stirring conditions, sulfuric acid with a concentration of 5% was added dropwise to adjust the pH to 3, and 15.5 g of dimethyldimethoxysilane was added. After sulfuric acid having a concentration of 5% was added dropwise to adjust the pH to 11, the reaction was carried out at 60 degrees for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain the powder of Example 2.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.19.
  • the powder was put into methyl ethyl ketone, and the intensity distribution was measured after irradiating with 500W ultrasonic waves for 3 minutes. It was found that D90 was 8 microns.
  • the specific surface area measured by the nitrogen adsorption method was 270 m 2 / g.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.086.
  • the powder was placed in methyl ethyl ketone, and the intensity distribution was measured after irradiating with 500W ultrasonic waves for 3 minutes.
  • the D90 was found to be 10 microns.
  • the specific surface area measured by the nitrogen adsorption method was 205 m 2 / g.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.086.
  • the powder was placed in methyl ethyl ketone, and the intensity distribution was measured after irradiating with 500W ultrasonic waves for 3 minutes.
  • the D90 was found to be 15 microns.
  • the specific surface area measured by the nitrogen adsorption method was 185 m 2 / g.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.086.
  • the powder was placed in methyl ethyl ketone, and the intensity distribution was measured after irradiating with 500W ultrasonic waves for 3 minutes.
  • the D90 was found to be 10 microns.
  • the specific surface area measured by the nitrogen adsorption method was 195 m 2 / g.
  • Water glass having a silica mass fraction of 30% was diluted with deionized water to an aqueous solution having a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel equipped with a heater and a stirrer.
  • the reaction system was heated to 100 degrees under stirring conditions, and the pH was adjusted to 9 by adding 5% sulfuric acid dropwise.
  • 4.2 g of dimethyldimethoxysilane was added and reacted at 100 ° C for 8 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain the powder of Example 6.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.051.
  • the powder was put into methyl ethyl ketone, and the intensity distribution was measured after being irradiated with a 500 W ultrasonic wave for 3 minutes. It was found that D90 was 19 micrometers.
  • the specific surface area measured by the nitrogen adsorption method was 190 m 2 / g.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees under stirring conditions, and the pH was adjusted to 9 by adding 5% sulfuric acid dropwise. 3.7 g of dimethyldimethoxysilane was added, and the reaction was carried out at 60 degrees for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain a powder of Comparative Example 1.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.045.
  • the powder was placed in methyl ethyl ketone, and the intensity distribution was measured after being irradiated with 500W ultrasonic waves for 3 minutes.
  • the D90 was found to be 75 microns.
  • the specific surface area measured by the nitrogen adsorption method was 200 m 2 / g.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees under stirring conditions, and the pH was adjusted to 9 by adding 5% sulfuric acid dropwise.
  • the reaction was carried out at 60 ° C for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain a powder of Comparative Example 2.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.
  • the powder was placed in methyl ethyl ketone, and the intensity distribution was measured after irradiating with 500W ultrasonic waves for 3 minutes. It was found that D90 could not be measured anymore, and a large number of millimeter-level agglomerates were found under microscope observation.
  • the specific surface area measured by the nitrogen adsorption method was 198 m 2 / g.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees under stirring conditions, and the pH was adjusted to 9 by adding 5% sulfuric acid dropwise. 20.6 g of dimethyldimethoxysilane was added and reacted at 60 ° C for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours. The dried solid was putty and could not be made into powder.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.25.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.086.
  • the powder was put into methyl ethyl ketone, and the intensity distribution was measured after being irradiated with a 500 W ultrasonic wave for 3 minutes.
  • the D90 was found to be 18 microns.
  • the specific surface area measured by the nitrogen adsorption method was 150 m 2 / g.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees under stirring conditions, and the pH was adjusted to 9 by adding 5% sulfuric acid dropwise.
  • 8.5 g of diphenyldimethoxysilane was added and reacted at 60 ° C for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain the powder of Example 8.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.05.
  • the powder was put into methyl ethyl ketone, and the intensity distribution was measured after being irradiated with a 500 W ultrasonic wave for 3 minutes.
  • the D90 was found to be 18 microns.
  • the specific surface area measured by the nitrogen adsorption method was 170 m 2 / g.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.085.
  • the powder was put into methyl ethyl ketone, and the intensity distribution was measured after being irradiated with a 500 W ultrasonic wave for 3 minutes. It was found that D90 was 19 micrometers.
  • the specific surface area measured by the nitrogen adsorption method was 175 m 2 / g.
  • the water glass with a silica mass fraction of 30% was diluted with deionized water to an aqueous solution with a silica mass fraction of 5%, and 1,000 grams were taken and placed in a reaction vessel with a heater and a stirrer.
  • the reaction system was heated to 60 degrees with stirring, and 4.5 g of dimethyldichlorosilane was added. Add 5% sulfuric acid to adjust the pH to 9.
  • the reaction was carried out at 60 ° C for 18 hours under stirring.
  • the reaction mixture was suction filtered, washed with deionized water and dried at 120 ° C for 3 hours.
  • the dried powder was dispersed with a high agitator for 3 minutes to obtain the powder of Example 10.
  • D unit / Q unit weight ratio measured by solid 29 SiNMR spectrometer 0.051.
  • the powder was placed in methyl ethyl ketone, and the intensity distribution was measured after being irradiated with 500W ultrasonic waves for 3 minutes.
  • the D90 was found to be 17 microns.
  • the specific surface area measured by the nitrogen adsorption method was 190 m 2 / g.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Polymers (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne une silice précipitée, qui est un siloxane constitué d'une unité D et d'une unité Q, l'unité D et l'unité Q étant présentes à un rapport pondéral de 0,05 à 0,19, l'unité Q étant du SiO 4- et l'unité D est du (CH 3) 2SiO 2-, (CH 3)HSiO 2-, H 2SiO 2-, (C 6H 5) 2SiO 2-, C 6H 5CH 3SiO 2-, C 6H 5HSiO 2-. L'invention concerne en outre un procédé de préparation de la silice précipitée, comprenant les étapes consistant à soumettre une substance dont l'unité Q est dérivée et une substance dont l'unité D est dérivée à une réaction de condensation avec de l'eau à un pH entre 8 et 11 pour générer un condensat, qui est rincé et séché pour obtenir la silice précipitée. L'incorporation de l'unité D dans la silice précipitée en plus de l'unité Q, couplée avec le contrôle du rapport pondéral de l'unité D à l'unité Q, peut résoudre le problème de dispersion de silice précipitée.
PCT/CN2018/098994 2018-08-06 2018-08-06 Nouvelle silice précipitée et son procédé de préparation WO2020029019A1 (fr)

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CN201880090624.3A CN111867974B (zh) 2018-08-06 2018-08-06 一种沉淀白炭黑及其制备方法
PCT/CN2018/098994 WO2020029019A1 (fr) 2018-08-06 2018-08-06 Nouvelle silice précipitée et son procédé de préparation

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CN116514131A (zh) * 2023-02-10 2023-08-01 山东弘兴白炭黑有限责任公司 一种用羟基硅油制备表面疏水型超细改性白炭黑的方法

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CN113905986B (zh) * 2021-09-07 2023-01-06 无锡恒诚硅业有限公司 一种粒径可控白炭黑的制备方法

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CN107697920A (zh) * 2017-11-21 2018-02-16 安徽伊法拉电气有限公司 一种采用溶胶‑凝胶法制备疏水型纳米白炭黑的方法

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CN1704452A (zh) * 2004-05-28 2005-12-07 河南大学 一种纳米二氧化硅微粒制备方法
CN102020285A (zh) * 2009-09-16 2011-04-20 深圳大学 一种疏水性二氧化硅气凝胶的制备方法
CN104355313A (zh) * 2014-08-06 2015-02-18 泉州三欣新材料科技有限公司 一种二氧化硅疏水多孔材料的简易制备方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116514131A (zh) * 2023-02-10 2023-08-01 山东弘兴白炭黑有限责任公司 一种用羟基硅油制备表面疏水型超细改性白炭黑的方法
CN116514131B (zh) * 2023-02-10 2024-01-23 山东弘兴白炭黑有限责任公司 一种用羟基硅油制备表面疏水型超细改性白炭黑的方法

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