CN107140645B - A kind of preparation method of the dedicated hydrated SiO 2 of engineering tyre - Google Patents
A kind of preparation method of the dedicated hydrated SiO 2 of engineering tyre Download PDFInfo
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- CN107140645B CN107140645B CN201710452068.7A CN201710452068A CN107140645B CN 107140645 B CN107140645 B CN 107140645B CN 201710452068 A CN201710452068 A CN 201710452068A CN 107140645 B CN107140645 B CN 107140645B
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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
- C01B33/126—Preparation of silica of undetermined type
- C01B33/128—Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
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- 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
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- 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
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of preparation methods of the dedicated hydrated SiO 2 of engineering tyre, which is characterized in that includes the following steps: that (1) sodium silicate solution of 0.1-0.2kg/L is added into reaction kettle, and stabilizer is added；(2) control mixing speed is 400-500r/min, is heated to 40-50 DEG C；(3) sulfuric acid solution of 0.04-0.05kg/L is added at one time into reaction system, reaction stood 2 hours after 4-5 hours；(4) dispersing agent is added into reaction system；(5) under mixing speed as described above, the sulfuric acid solution of 0.04-0.05kg/L is added dropwise into reaction system, is reacted 5-6 hours at 50-60 DEG C；(6) above-mentioned to be warming up to 90-95 DEG C after reaction and cure 2 hours, washing, filters pressing, dry hydrated SiO 2.The hydrated SiO 2 as made from the method for the invention, good with rubber compatibility, reinforcing effect is high.
Description
Technical field
The present invention relates to chemical industry manufacturing fields, and in particular to a kind of preparation side of the dedicated hydrated SiO 2 of engineering tyre
Method.
Background technique
In recent years, domestic and international project construction and transporting equipment used in Mining Market were increasingly enlarged, this causes to work
Journey is mechanical and its tire delivers load and performance requirement is more harsh.
Compared with conventional tyre, due to the load weight of engineering truck, engineering tyre needs to have more excellent wearability, i.e.,
Surface of tyre is not easy to wear.With the development of industry, the requirement to engineering tyre high performance also improves year by year, and this requires wheels
Tire tread has excellent wearability.
On the other hand, from last century the nineties, white carbon black is widely used in tire tread formula as reinforced filling,
Obtaining the properties of above-mentioned tire tread requirement significantly improves.However, introducing the rubber of silica at present
The wearability and reinforcing effect of composition are still reached to less than satisfactory degree, to find out its cause, silica and rubber
Compatibility is poor, thus reinforcing effect is caused to be not enough.
Summary of the invention
For above-mentioned status, the present invention provides a kind of preparation method of dedicated hydrated SiO 2 of engineering tyre.Pass through this
The compatibility of hydrated SiO 2 made from the preparation method of invention and rubber is good, and reinforcing effect is especially abundant, can be used for engineering
The preparation of wheel tire, it may be said that be a kind of dedicated hydrated SiO 2 of engineering tyre.
Specifically, the present invention provides a kind of preparation method of dedicated hydrated SiO 2 of engineering tyre comprising Xia Shubu
It is rapid:
(1) sodium silicate solution of 0.1-0.2kg/L is added into reaction kettle, and stabilizer is added；
(2) control mixing speed is 400-500r/min, is heated to 40-50 DEG C；
(3) sulfuric acid solution of 0.04-0.05kg/L is added at one time into reaction system, reaction stood 30 after 2-3 hours
Minute；
(4) dispersing agent is added into reaction system；
(5) under mixing speed as described above, the sulfuric acid solution of 0.04-0.05kg/L, 50- are added dropwise into reaction system
It is reacted 5-6 hours at 60 DEG C；
(6) above-mentioned to be warming up to 90-95 DEG C after reaction and cure 2 hours, washing, filters pressing, dry hydrated SiO 2.
Wherein, the stabilizer is one of hydroquinone or polyvinylpyrrolidone.
In addition, the stabilizer is the 2-5% of sodium metasilicate weight.
In addition, in step (3), the volume ratio of sodium silicate solution and sulfuric acid solution is 1:0.8-1.
In addition, the dispersing agent is one of lauryl sodium sulfate, sodium citrate or p-methyl benzenesulfonic acid sodium.
In addition, the dispersing agent is the 1-2% of sodium metasilicate weight.
In addition, the ratio of the total volume of the sulfuric acid solution of original sodium silicate solution and dropwise addition is 1:0.4- in step (5)
0.6, rate of addition 0.5L/h.
The present invention, by the way that sulfuric acid is added in batches, and control reaction condition and during the reaction be added stabilizer and
Dispersing agent, can prepare a kind of and good hydrated SiO 2 of rubber compatibility, and the reinforcing height of the hydrated SiO 2 can be used
It is a kind of dedicated hydrated SiO 2 of engineering tyre in engineering tyre.
Specific embodiment
The present invention is described in detail below with reference to embodiment, but the present invention is not limited to these embodiments, in this field
The replacement of customary means, is all contained in the scope of the invention in range.
Embodiment 1
(1) 1L mass concentration is added into reaction kettle and is the sodium silicate solution of 0.1kg/L, and 2g hydroquinone is added；
(2) control mixing speed is 400r/min, is heated to 40 DEG C；
(3) sulfuric acid solution that 0.8L mass concentration is 0.04kg/L is added at one time into reaction system, after reaction 2 hours
Stand 30 minutes；
(4) 1g lauryl sodium sulfate is added into reaction system；
(5) under mixing speed as described above, it is molten that the sulfuric acid that mass concentration is 0.04kg/L is added dropwise into reaction system
Liquid total 0.4L, rate of addition 0.5L/h react 5 hours at 50 DEG C；
(6) above-mentioned to be warming up to 90 DEG C after reaction and cure 2 hours, washing, filters pressing, dry hydrated SiO 2.It presses
According to the specific surface area 200.5m of GB/T3073-1999 measurement hydrated SiO 22/g。
Embodiment 2
(1) 1L mass concentration is added into reaction kettle and is the sodium silicate solution of 0.2kg/L, and 6g polyvinylpyrrolidine is added
Alkanone；
(2) control mixing speed is 500r/min, is heated to 50 DEG C；
(3) sulfuric acid solution that 1L mass concentration is 0.05kg/L is added at one time into reaction system, it is quiet after reaction 3 hours
It sets 30 minutes；
(4) 4g sodium citrate is added into reaction system；
(5) under mixing speed as described above, it is molten that the sulfuric acid that mass concentration is 0.05kg/L is added dropwise into reaction system
Liquid total 0.6L, rate of addition 0.5L/h react 5 hours at 60 DEG C；
(6) above-mentioned to be warming up to 95 DEG C after reaction and cure 2 hours, washing, filters pressing, dry hydrated SiO 2.It presses
According to the specific surface area 205.3m of GB/T3073-1999 measurement hydrated SiO 22/g。
Embodiment 3
(1) 1L mass concentration is added into reaction kettle and is the sodium silicate solution of 0.1kg/L, and 5g hydroquinone is added；
(2) control mixing speed is 450r/min, is heated to 45 DEG C；
(3) sulfuric acid solution that 0.9L mass concentration is 0.04kg/L is added at one time into reaction system, after reaction 2 hours
Stand 30 minutes；
(4) 2g p-methyl benzenesulfonic acid sodium is added into reaction system；
(5) under mixing speed as described above, it is molten that the sulfuric acid that mass concentration is 0.04kg/L is added dropwise into reaction system
Liquid total 0.5L, rate of addition 0.5L/h react 5 hours at 55 DEG C；
(6) above-mentioned to be warming up to 95 DEG C after reaction and cure 2 hours, washing, filters pressing, dry hydrated SiO 2.It presses
According to the specific surface area 203.9m of GB/T3073-1999 measurement hydrated SiO 22/g。
Hydrated SiO 2 made from embodiment 1-3 and butadiene-styrene rubber and promotor, coupling agent etc. are mixed by a certain percentage
It is smelt tire tread glue, then high temperature vulcanized molding.It is tried using AKRON abrasion wear test machine (GT-7012-A), computer system pulling force
Test hardness, tensile strength, the tearing strength of the instrument tests tread rubbers such as machine (GT-TCS-2000), durometer (GT-706N)
Etc. physical properties.The results are shown in Table 1.
Table 1
As shown in Table 1, the compatibility of hydrated SiO 2 and rubber produced by the present invention is good, easily disperse, it is reinforcing more
It is excellent, it can especially be used for the filler of engineering tyre.
Claims (5)
1. a kind of preparation method of the dedicated hydrated SiO 2 of engineering tyre, which is characterized in that include the following steps:
(1) sodium silicate solution of 0.1-0.2kg/L is added into reaction kettle, and stabilizer is added；
(2) control mixing speed is 400-500r/min, is heated to 40-50 DEG C；
(3) the sulfuric acid solution 0.8-1.0L of 0.04-0.05kg/L is added at one time into reaction system, it is quiet after reaction 2-3 hours
It sets 30 minutes；
(4) dispersing agent is added into reaction system；
(5) under mixing speed as described above, the sulfuric acid solution 0.4- of 0.04-0.05kg/L is added dropwise into reaction system
It is reacted 5-6 hours at 0.6L, 50-60 DEG C；
(6) above-mentioned to be warming up to 90-95 DEG C after reaction and cure 2 hours, washing, filters pressing, dry hydrated SiO 2；
The stabilizer is one of hydroquinone or polyvinylpyrrolidone, and the dispersing agent is dodecyl sulphate
One of sodium, sodium citrate or p-methyl benzenesulfonic acid sodium.
2. preparation method according to claim 1, which is characterized in that the stabilizer is the 2-5% of sodium metasilicate weight.
3. preparation method according to claim 1, which is characterized in that in step (3), sodium silicate solution and sulfuric acid solution
Volume ratio be 1:0.8-1.
4. preparation method according to claim 1, which is characterized in that the dispersing agent is the 1-2% of sodium metasilicate weight.
5. preparation method according to claim 1, which is characterized in that in step (5), original sodium silicate solution and dropwise addition
Sulfuric acid solution total volume ratio be 1:0.4-0.6, rate of addition 0.5L/h.
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| CN107140645B true CN107140645B (en) | 2019-08-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1313370C (en) * | 2005-01-07 | 2007-05-02 | 安徽工业大学 | Method for preparing hydrated silicon dioxide |
| CN101774591B (en) * | 2010-02-26 | 2012-06-27 | 无锡恒诚硅业有限公司 | Production technology of white microsphere high-strength white carbon black |
| CN102964881B (en) * | 2012-12-07 | 2015-04-08 | 北京彤程创展科技有限公司 | Amino/mercapto silane modified silica and preparation method thereof |
| CN103435046B (en) * | 2013-08-06 | 2015-08-05 | 龙星化工股份有限公司 | A kind of manufacture craft of high-dispersity white carbon black of snow tire |
| CN104176739B (en) * | 2014-08-18 | 2016-09-21 | 连云港市东海县宏伟石英制品有限公司 | A kind of sodium silicate prepares the method for high-purity silicon dioxide powder |
| CN106744988A (en) * | 2015-11-25 | 2017-05-31 | 衡阳市锦轩化工有限公司 | A kind of preparation method of high-quality precipitated hydrated silica |
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