CN104891506A - Manufacturing method of low-BET high-dispersivity silica white - Google Patents

Abstract

The invention provides a manufacturing method of low-BET high-dispersivity silica white, which comprises the following steps: (1) preparing a Na2SiO3 solution and a sodium sulfate solution; (2) heating the Na2SiO3 solution to 80-100 DEG C, adding the sodium sulfate solution, and neutralizing with concentrated sulfuric acid until the pH value is 9-11; continuing adding the sulfuric acid solution, and stirring to react for 50-70 minutes until the pH value is 6-7; (3) cooling to 60-70 DEG C, and aging for 30-40 minutes to obtain a slurry; (4) cooling the slurry to 40-60 DEG C, regulating the pH value to 2-5, carrying out pressure filtration, and washing to obtain a wet filter cake; and (5) dispersing the wet filter cake obtained in the step (4) in an acetone water solution, heating while stirring, refluxing, carrying out vacuum filtration, and drying to obtain the silica white. The silica white prepared by the method has favorable dispersivity and higher ice surface gripping power (by 6%), and can satisfy the requirements of ice tires for high-dispersivity silica white.

Description

A kind of manufacture method of low BET high-dispersity white carbon black

Technical field

The present invention relates to a kind of manufacture method of low BET high-dispersity white carbon black.

Background technology

White carbon black is the general name of white powder X-ray amorphous silicic acid and silicate product, mainly refers to precipitated silica, aerosil, superfine silicon dioxide gel and aerogel, also comprises Powdered synthetic aluminium silicate and Calucium Silicate powder etc.White carbon black is porous material, and it forms available SiO ₂nH ₂o represents, wherein nH ₂o exists with the form of surface hydroxyl.White carbon black can be dissolved in caustic alkali and hydrofluoric acid, the acid beyond water insoluble, solvent and hydrofluoric acid, have high temperature resistant, do not fire, tasteless, odorless, good electrical insulating property.White carbon black, as the auxiliary agent of a kind of environmental protection, excellent performance, is mainly used in rubber item (comprising high-temperature silicon disulfide rubber), weaving, papermaking, agricultural chemicals, foodstuff additive field.

Summary of the invention

The invention provides a kind of manufacture method of low BET high-dispersity white carbon black, apply the white carbon black good dispersity that method of the present invention prepares, be applicable to snow tire.

The invention provides a kind of manufacture method of low BET high-dispersity white carbon black, step is as follows:

(1) Na of 0.4-0.6mol/L is prepared ₂siO ₃the metabisulfite solution of solution and 1-2mol/L;

(2) by Na prepared by step (1) ₂siO ₃solution warms, to 80-100 DEG C, adds metabisulfite solution, and add-on is Na ₂siO ₃the 0.1-0.2% of liquor capacity; Neutralize with the vitriol oil, terminal pH is 9-11; Continue to add the sulphuric acid soln stirring reaction 50-70min that concentration is 2-4mol/L, terminal pH is 6-7;

(3) be cooled to 60-70 DEG C, aging 30-40min, wherein, stir speed (S.S.) is 15rpm-20rpm, obtains slurries;

(4) after slurries being cooled to 40-60 DEG C, adjust pH to 2-5, press filtration, washing obtain wet cake;

(5) be scattered in the aqueous solution of acetone by the wet cake that step (4) obtains, wherein the concentration of acetone is 1.5-1.8mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.

Metabisulfite solution add the dispersiveness that can improve white carbon black, wet cake is dissolved in process in the aqueous solution of acetone and can improves the dispersiveness of white carbon black further, with do not add metabisulfite solution and compare without the preparation method of aqueous acetone solution process wet cake, the hard charcoal black ice face gripping power that the inventive method prepares improves 6%, can meet the requirement of snow tire to high-dispersion white carbon black.

Accompanying drawing explanation

Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:

Fig. 1 is the process flow sheet of preparation method of the present invention.

Embodiment

Following embodiment is convenient to understand the present invention better, but does not limit the present invention.Experimental technique in following embodiment, if no special instructions, is ordinary method.

embodiment 1

The manufacture method step of low BET high-dispersity white carbon black of the present invention is as follows:

(1) Na of 0.5mol/L is prepared ₂siO ₃the metabisulfite solution of solution and 1.5mol/L;

(2) by Na prepared by step (1) ₂siO ₃solution warms to 90 DEG C, adds metabisulfite solution, and add-on is Na ₂siO ₃0.15% of liquor capacity; Neutralize with the vitriol oil, terminal pH is 10; Continue to add the sulphuric acid soln stirring reaction 60min that concentration is 3mol/L, terminal pH is 6.5;

(3) be cooled to 65 DEG C, aging 35min, wherein, stir speed (S.S.) is 18rpm, obtains slurries;

(4) after slurries being cooled to 50 DEG C, adjust pH to 3, press filtration, washing obtain wet cake;

(5) be scattered in the aqueous solution of acetone by the wet cake that step (4) obtains, wherein the concentration of acetone is 1.6mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.

embodiment 2

The manufacture method step of low BET high-dispersity white carbon black of the present invention is as follows:

(1) Na of 0.4mol/L is prepared ₂siO ₃the metabisulfite solution of solution and 2mol/L;

(2) by Na prepared by step (1) ₂siO ₃solution warms to 100 DEG C, adds metabisulfite solution, and add-on is Na ₂siO ₃0.1% of liquor capacity; Neutralize with the vitriol oil, terminal pH is 11; Continue to add the sulphuric acid soln stirring reaction 50min that concentration is 2mol/L, terminal pH is 7;

(3) be cooled to 60 DEG C, aging 40min, wherein, stir speed (S.S.) is 15rpm, obtains slurries;

(4) after slurries being cooled to 60 DEG C, adjust pH to 2, press filtration, washing obtain wet cake;

(5) be scattered in the aqueous solution of acetone by the wet cake that step (4) obtains, wherein the concentration of acetone is 1.5mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.

embodiment 3

The manufacture method step of low BET high-dispersity white carbon black of the present invention is as follows:

(1) Na of 0.6mol/L is prepared ₂siO ₃the metabisulfite solution of solution and 1mol/L;

(2) by Na prepared by step (1) ₂siO ₃solution warms to 80 DEG C, adds metabisulfite solution, and add-on is Na ₂siO ₃0.2% of liquor capacity; Neutralize with the vitriol oil, terminal pH is 9; Continue to add the sulphuric acid soln stirring reaction 70min that concentration is 4mol/L, terminal pH is 6;

(3) be cooled to 70 DEG C, aging 30min, wherein, stir speed (S.S.) is 20rpm, obtains slurries;

(4) after slurries being cooled to 40 DEG C, adjust pH to 5, press filtration, washing obtain wet cake;

(5) be scattered in the aqueous solution of acetone by the wet cake that step (4) obtains, wherein the concentration of acetone is 1.8mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.

Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (1)

1. a manufacture method for low BET high-dispersity white carbon black, is characterized in that: step is as follows:

(1) Na of 0.4-0.6mol/L is prepared ₂siO ₃the metabisulfite solution of solution and 1-2mol/L;

(2) by Na prepared by step (1) ₂siO ₃solution warms, to 80-100 DEG C, adds metabisulfite solution, and add-on is Na ₂siO ₃the 0.1-0.2% of liquor capacity; Neutralize with the vitriol oil, terminal pH is 9-11; Continue to add the sulphuric acid soln stirring reaction 50-70min that concentration is 2-4mol/L, terminal pH is 6-7;

(3) be cooled to 60-70 DEG C, aging 30-40min, wherein, stir speed (S.S.) is 15rpm-20rpm, obtains slurries;

(4) after slurries being cooled to 40-60 DEG C, adjust pH to 2-5, press filtration, washing obtain wet cake;

(5) be scattered in the aqueous solution of acetone by the wet cake that step (4) obtains, wherein the concentration of acetone is 1.5-1.8mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.