CN100406379C - Deacidification method for vapor process of preparing nano SiO2 - Google Patents
Deacidification method for vapor process of preparing nano SiO2 Download PDFInfo
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- CN100406379C CN100406379C CNB031169473A CN03116947A CN100406379C CN 100406379 C CN100406379 C CN 100406379C CN B031169473 A CNB031169473 A CN B031169473A CN 03116947 A CN03116947 A CN 03116947A CN 100406379 C CN100406379 C CN 100406379C
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- depickling
- fluidisation
- gas
- fluidizing
- sio2
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Abstract
The present invention discloses a deacidifying method for preparing nanometer silicon dioxide (SiO2) by a gas phase method. In the method, mixed gas after the combustion of hydrogen gas and the air is used as fluidizing gas; nanometer SiO2 is deacidified in a fluidized-bed reactor; the fluidizing deacidifying temperature is from 300 DEG C to 500 DEG C, and the speed of the fluidizing gas is from 2 cm/s to 15 cm/s. After the nanometer SiO2 is deacidified, the pH value of the nanometer SiO2 is greater than 4; the water content is smaller than 2%.
Description
Technical field
The present invention relates to a kind of acid stripping method, specifically, relate to a kind of preparing nano silicon dioxide by vapor phase process (SiO that is used for
2) acid stripping method.
Background technology
The nanometer SiO of vapor phase process preparation
2It is a kind of high-tech inorganic fine chemical product, because the peculiar character of nano material, it is widely used in many industrial circles such as rubber, coating, tackiness agent, makeup, printing ink, plastics, medicine, is the very wide nano material of a kind of development prospect.
Vapor phase process prepares nanometer SiO
2Be by silicon tetrachloride (SiCl
4) make through high-temperature hydrolysis, its reaction formula is as follows:
SiCl
4+2H
2O→SiO
2+4HCl
By above-mentioned reaction formula as can be known, follow SiO
2Generation, have a large amount of hydrogenchloride (HCl) gas to produce simultaneously.Nanometer SiO
2Be the powder that a kind of particle diameter is very little, specific surface is very big, thereby in its preparation process, adsorbed a large amount of HCl.And at nanometer SiO
2(being commonly called as white carbon black) major applications occasion (as silicon rubber etc.), it is a leading indicator of measurement quality product that the remaining HCl amount of white carbon black absorption is had strict demand, its pH value.In addition, in above-mentioned reaction, reactants water steam is excessive, and the white carbon black product has also adsorbed many moisture content, and in order to satisfy the requirement of various application scenarios, institute's water content also must be removed in the lump with HCl, to reach the planned quality of the product standard-required.
In the thermal silica production process, nanometer SiO
2Depickling generally has two kinds of methods.A kind of is that the dry air that will be preheating to certain temperature feeds in the extracting tower and SiO
2Gas-solid two-phase mass transfer is carried out in the powder contact; Another kind is to add NH in dry air
3, remove HCl by chemical action.A kind of acid stripping method in back is introduced impurity artificially, influences quality product; And first method is undesirable through facts have proved its deacidification effect.
Summary of the invention
The object of the invention is, a kind of nanometer SiO that removes the vapor phase process preparation is provided
2The method of absorption HCl makes nanometer SiO
2PH greater than 4.0 and water content less than 2%.
The object of the present invention is achieved like this:
It is fluidizing agent that the present invention adopts the mixed gas after hydrogen and the air combustion, in fluidized-bed reactor to nanometer SiO
2Carry out depickling, wherein the volume ratio of hydrogen and air preferred 1: 2～20, and the temperature of fluidisation depickling is 300～500 ℃, and fluidizing gas velocity is 2～15cm/s, and the fluidisation rate of expansion is 3～6, and the time of fluidisation depickling is 30～90min.
The method of depickling of the present invention and water has compared with prior art that gas-solid two-phase contact condition is good, and the depickling time is fast, does not need to add in addition moisture content, can not introduce other impurity, compares advantages such as can sharply not increasing resistance with fixed bed.
Embodiment
The invention will be further described below by embodiment, and the cited case does not limit protection scope of the present invention:
Embodiment 1
Earlier with fluidized gas (H
2With the volume ratio of air be 1: 20) be preheated to 600～700 ℃, pass the uniform back of porcelain ring then and arrive the nanometer SiO of fluidisation section adding by fluidization column top
2Carry out the fluidisation depickling, the temperature of fluidisation depickling is 300 ℃, and fluidizing gas velocity is 5cm/s, and the fluidisation rate of expansion is 3, the nanometer SiO after fluidisation depickling in 30 minutes
2By fluidization column bottom discharge hole for discharge, carry out product analysis.
The product analysis result:
Before the depickling: nanometer SiO
2PH:2.50, contain H
2O:2.0%, specific surface area 201m
2/ g;
After the depickling: nanometer SiO
2PH:4.19, contain H
2O:1.0%, specific surface area 200m
2/ g.
Embodiment 2
Earlier with fluidized gas (H
2With the volume ratio of air be 1: 10) be preheated to 600～700 ℃, pass the uniform back of porcelain ring then and arrive the nanometer SiO of fluidisation section adding by fluidization column top
2Carry out the fluidisation depickling, the temperature of fluidisation depickling is 500 ℃, and fluidizing gas velocity is 15cm/s, and the fluidisation rate of expansion is 6, the nanometer SiO after fluidisation depickling in 90 minutes
2By fluidization column bottom discharge hole for discharge, carry out product analysis.
The product analysis result:
Before the depickling: nanometer SiO
2PH:1.90, contain H
2O:4.6%, specific surface area 460m
2/ g;
After the depickling: nanometer SiO
2PH:4.26, contain H
2O:2.0%, specific surface area 459m
2/ g.
Claims (2)
1. an acid stripping method that is used for preparing nano silicon dioxide by vapor phase process is characterized in that, the key step of said method is a fluidizing agent for adopting the mixed gas after hydrogen and the air combustion, in fluidized-bed reactor to nanometer SiO
2Carry out depickling and dehydration, fluidizing gas velocity is 2～15cm/s, and the temperature of fluidisation depickling is 300～500 ℃, and the fluidisation rate of expansion is 3～6, and the time of fluidisation depickling and water is 30～90min; Wherein the volume ratio of hydrogen and air is 1: 2～20.
2. method as claimed in claim 2 is characterized in that, wherein said fluidizing agent is preheated to 600～700 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031169473A CN100406379C (en) | 2003-05-16 | 2003-05-16 | Deacidification method for vapor process of preparing nano SiO2 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031169473A CN100406379C (en) | 2003-05-16 | 2003-05-16 | Deacidification method for vapor process of preparing nano SiO2 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1548370A CN1548370A (en) | 2004-11-24 |
| CN100406379C true CN100406379C (en) | 2008-07-30 |
Family
ID=34320539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031169473A Expired - Lifetime CN100406379C (en) | 2003-05-16 | 2003-05-16 | Deacidification method for vapor process of preparing nano SiO2 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100406379C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431955C (en) * | 2006-09-04 | 2008-11-12 | 上海氯碱化工股份有限公司 | Apparatus and method of synthesizing acidic material on SiO2 surface by eliminating gas phase method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1208016A (en) * | 1998-08-27 | 1999-02-17 | 沈阳化工股份有限公司 | Gas phase process preparing white carbon |
-
2003
- 2003-05-16 CN CNB031169473A patent/CN100406379C/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1208016A (en) * | 1998-08-27 | 1999-02-17 | 沈阳化工股份有限公司 | Gas phase process preparing white carbon |
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|---|---|
| CN1548370A (en) | 2004-11-24 |
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Granted publication date: 20080730 |