CN107140645A - A kind of preparation method of the special hydrated SiO 2 of engineering tyre - Google Patents
A kind of preparation method of the special hydrated SiO 2 of engineering tyre Download PDFInfo
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- CN107140645A CN107140645A CN201710452068.7A CN201710452068A CN107140645A CN 107140645 A CN107140645 A CN 107140645A CN 201710452068 A CN201710452068 A CN 201710452068A CN 107140645 A CN107140645 A CN 107140645A
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- sulfuric acid
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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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Silicon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of the special hydrated SiO 2 of engineering tyre, it is characterised in that comprises the steps：（1）0.1 0.2kg/L sodium silicate solution is added into reactor, and adds stabilizer；（2）It is 400 500r/min to control mixing speed, is heated to 40 50 DEG C；（3）The disposable sulfuric acid solution for adding 0.04 0.05kg/L into reaction system, reaction stands 2 hours after 45 hours；（4）Dispersant is added into reaction system；（5）Under mixing speed as described above, it is added dropwise at 0.04 0.05kg/L sulfuric acid solution, 50 60 DEG C and reacts 56 hours into reaction system；（6）Above-mentioned reaction is warming up to 90 95 DEG C and cured 2 hours after terminating, washing, press filtration, 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
Field is manufactured the present invention relates to chemical industry, and in particular to a kind of preparation side of the special hydrated SiO 2 of engineering tyre
Method.
Background technology
In recent years, transporting equipment used in domestic and international project construction and Mining Market maximized increasingly, and this causes to work
Journey machinery and its tire delivery load and performance requirement are more harsh.
Compared with conventional tyre, due to the load weight of engineering truck, engineering tyre needs have more excellent wearability, i.e.,
Surface of tyre is not easy to wear.With industrial expansion, the requirement to engineering tyre high performance is also improved year by year, and this requires wheel
Tire tread has excellent wearability.
On the other hand, from last century the nineties, white carbon is widely used in tire tread formula as reinforced filling,
The properties of above-mentioned tire tread requirement are made to obtain obvious improve.However, introducing the rubber of silica at present
The wearability and enhancing effect of composition are still reached to less than gratifying degree, to find out its cause, silica and rubber
Compatibility is poor, thus causes reinforcing effect not abundant enough.
The content of the invention
For above-mentioned present situation, the present invention provides a kind of preparation method of the special hydrated SiO 2 of engineering tyre.By this
The compatibility of hydrated SiO 2 and rubber is good made from the preparation method of invention, and reinforcing effect is especially abundant, available for engineering
The preparation of wheel tire, it may be said that be a kind of special hydrated SiO 2 of engineering tyre.
Specifically, the present invention provides a kind of preparation method of the special hydrated SiO 2 of engineering tyre, and it includes following steps
Suddenly：
（1）0.1-0.2kg/L sodium silicate solution is added into reactor, and adds stabilizer；
（2）It is 400-500r/min to control mixing speed, is heated to 40-50 DEG C；
（3）The disposable sulfuric acid solution for adding 0.04-0.05kg/L into reaction system, reaction stands 30 minutes after 2-3 hours；
（4）Dispersant is added into reaction system；
（5）Under mixing speed as described above, 0.04-0.05kg/L sulfuric acid solution, 50-60 DEG C are added dropwise into reaction system
Lower reaction 5-6 hours；
（6）Above-mentioned reaction is warming up to 90-95 DEG C and cured 2 hours after terminating, washing, press filtration, dry hydrated SiO 2.
Wherein, the stabilizer is one kind in hydroquinones or PVP.
In addition, the stabilizer is the 2-5% of sodium metasilicate weight.
In addition, in step（3）In, the volume ratio of sodium silicate solution and sulfuric acid solution is 1:0.8-1.
In addition, the dispersant is one kind in lauryl sodium sulfate, sodium citrate or p-methyl benzenesulfonic acid sodium.
In addition, the dispersant is the 1-2% of sodium metasilicate weight.
In addition, in step（5）In, the ratio of original sodium silicate solution and the cumulative volume for the sulfuric acid solution being added dropwise is 1:0.4-
0.6, rate of addition is 0.5L/h.
The present invention, by adding sulfuric acid in batches, and control reaction condition and add during the course of the reaction stabilizer and
Dispersant, 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 special hydrated SiO 2 of engineering tyre in engineering tyre.
Embodiment
The present invention is described in detail with reference to embodiment, but the present invention is not limited to these embodiments, in this area
In the range of customary means replacement, be all contained in the scope of the invention.
Embodiment 1
（1）1L mass concentrations are added into reactor and are 0.1kg/L sodium silicate solution, and add 2g hydroquinones；
（2）It is 400r/min to control mixing speed, is heated to 40 DEG C；
（3）Disposable into reaction system to add the sulfuric acid solution that 0.8L mass concentrations are 0.04kg/L, reaction is stood after 2 hours
30 minutes；
（4）1g lauryl sodium sulfate is added into reaction system；
（5）Under mixing speed as described above, mass concentration is added dropwise into reaction system and is total to for 0.04kg/L sulfuric acid solution
0.4L, rate of addition is 0.5L/h, is reacted 5 hours at 50 DEG C；
（6）Above-mentioned reaction is warming up to 90 DEG C and cured 2 hours after terminating, washing, press filtration, dry hydrated SiO 2.According to GB/
T3073-1999 determines the specific surface area 200.5m of hydrated SiO 22/g。
Embodiment 2
（1）1L mass concentrations are added into reactor and are 0.2kg/L sodium silicate solution, and add 6g polyvinylpyrrolidones
Ketone；
（2）It is 500r/min to control mixing speed, is heated to 50 DEG C；
（3）Disposable into reaction system to add the sulfuric acid solution that 1L mass concentrations are 0.05kg/L, reaction stands 30 after 3 hours
Minute；
（4）4g sodium citrates are added into reaction system；
（5）Under mixing speed as described above, mass concentration is added dropwise into reaction system and is total to for 0.05kg/L sulfuric acid solution
0.6L, rate of addition is 0.5L/h, is reacted 5 hours at 60 DEG C；
（6）Above-mentioned reaction is warming up to 95 DEG C and cured 2 hours after terminating, washing, press filtration, dry hydrated SiO 2.According to GB/
T3073-1999 determines the specific surface area 205.3m of hydrated SiO 22/g。
Embodiment 3
（1）1L mass concentrations are added into reactor and are 0.1kg/L sodium silicate solution, and add 5g hydroquinones；
（2）It is 450r/min to control mixing speed, is heated to 45 DEG C；
（3）Disposable into reaction system to add the sulfuric acid solution that 0.9L mass concentrations are 0.04kg/L, reaction is stood after 2 hours
30 minutes；
（4）2g p-methyl benzenesulfonic acid sodium is added into reaction system；
（5）Under mixing speed as described above, mass concentration is added dropwise into reaction system and is total to for 0.04kg/L sulfuric acid solution
0.5L, rate of addition is 0.5L/h, is reacted 5 hours at 55 DEG C；
（6）Above-mentioned reaction is warming up to 95 DEG C and cured 2 hours after terminating, washing, press filtration, dry hydrated SiO 2.According to GB/
T3073-1999 determines the specific surface area 203.9m of hydrated SiO 22/g。
Hydrated SiO 2 made from embodiment 1-3 and butadiene-styrene rubber and accelerator, coupling agent etc. are mixed by a certain percentage
Tire tread glue is smelt, then high temperature vulcanized shaping.Using AKRON abrasion wear test machines（GT-7012-A）, computer system pulling force examination
Test machine（GT-TCS-2000）, durometer（GT-706N）Deng the hardness, tensile strength, tearing strength of instrument test tread rubber
Etc. physical property.As a result it is as 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 scattered, reinforcing more excellent,
The filler of engineering tyre can especially be used it for.
Claims (7)
1. a kind of preparation method of the special hydrated SiO 2 of engineering tyre, it is characterised in that comprise the steps：
（1）0.1-0.2kg/L sodium silicate solution is added into reactor, and adds stabilizer；
（2）It is 400-500r/min to control mixing speed, is heated to 40-50 DEG C；
（3）The disposable sulfuric acid solution for adding 0.04-0.05kg/L into reaction system, reaction stands 30 minutes after 2-3 hours；
（4）Dispersant is added into reaction system；
（5）Under mixing speed as described above, 0.04-0.05kg/L sulfuric acid solution, 50-60 DEG C are added dropwise into reaction system
Lower reaction 5-6 hours；
（6）Above-mentioned reaction is warming up to 90-95 DEG C and cured 2 hours after terminating, washing, press filtration, dry hydrated SiO 2.
2. preparation method according to claim 1, it is characterised in that the stabilizer is hydroquinones or polyvinyl pyrrole
One kind in pyrrolidone.
3. preparation method according to claim 1 or 2, it is characterised in that the stabilizer is the 2-5% of sodium metasilicate weight.
4. preparation method according to claim 1, it is characterised in that in step（3）In, sodium silicate solution and sulfuric acid solution
Volume ratio be 1:0.8-1.
5. preparation method according to claim 1, it is characterised in that the dispersant is lauryl sodium sulfate, lemon
One kind in sour sodium or p-methyl benzenesulfonic acid sodium.
6. preparation method according to claim 5, it is characterised in that the dispersant is the 1-2% of sodium metasilicate weight.
7. preparation method according to claim 1, it is characterised in that in step（5）In, original sodium silicate solution is with being added dropwise
Sulfuric acid solution cumulative volume ratio be 1:0.4-0.6, rate of addition is 0.5L/h.
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| CN201710452068.7A CN107140645B (en) | 2017-06-15 | 2017-06-15 | A kind of preparation method of the dedicated hydrated SiO 2 of engineering tyre |
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| CN107140645B CN107140645B (en) | 2019-08-23 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648042A (en) * | 2005-01-07 | 2005-08-03 | 安徽工业大学 | Method for preparing hydrated silicon dioxide |
| CN101774591A (en) * | 2010-02-26 | 2010-07-14 | 无锡恒诚硅业有限公司 | Production technology of white microsphere high-strength white carbon black |
| CN102964881A (en) * | 2012-12-07 | 2013-03-13 | 北京彤程创展科技有限公司 | Amino/mercapto silane modified silica and preparation method thereof |
| CN103435046A (en) * | 2013-08-06 | 2013-12-11 | 龙星化工股份有限公司 | Preparation technology of high-dispersity white carbon black for snow tire |
| CN104176739A (en) * | 2014-08-18 | 2014-12-03 | 连云港市东海县宏伟石英制品有限公司 | Method for preparing high-purity silicon dioxide powder by using sodium silicate |
| 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 |
-
2017
- 2017-06-15 CN CN201710452068.7A patent/CN107140645B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648042A (en) * | 2005-01-07 | 2005-08-03 | 安徽工业大学 | Method for preparing hydrated silicon dioxide |
| CN101774591A (en) * | 2010-02-26 | 2010-07-14 | 无锡恒诚硅业有限公司 | Production technology of white microsphere high-strength white carbon black |
| CN102964881A (en) * | 2012-12-07 | 2013-03-13 | 北京彤程创展科技有限公司 | Amino/mercapto silane modified silica and preparation method thereof |
| CN103435046A (en) * | 2013-08-06 | 2013-12-11 | 龙星化工股份有限公司 | Preparation technology of high-dispersity white carbon black for snow tire |
| CN104176739A (en) * | 2014-08-18 | 2014-12-03 | 连云港市东海县宏伟石英制品有限公司 | Method for preparing high-purity silicon dioxide powder by using sodium silicate |
| 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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