CN107021495A - A kind of preparation method of the rubber high reinforcing silica of high oil absorption - Google Patents
A kind of preparation method of the rubber high reinforcing silica of high oil absorption Download PDFInfo
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- CN107021495A CN107021495A CN201710287776.XA CN201710287776A CN107021495A CN 107021495 A CN107021495 A CN 107021495A CN 201710287776 A CN201710287776 A CN 201710287776A CN 107021495 A CN107021495 A CN 107021495A
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- preparation
- oil absorption
- rubber
- stirring
- reinforcing silica
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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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/142—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates
- C01B33/143—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates
-
- 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)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of rubber with the high reinforcing silica of high oil absorption, the first accurate formulation waterglass in make-up tank；Enter reactor from change a job skill hot water, the glass that adds water from refinery pit of warm water tank again, be warming up to 60 DEG C；While stirred on one side toward sulfuric acid and dilution water is added in reactor, stop stirring and be aged 30 minutes after pH is controlled between 6.5 ~ 7.0；Start stirring, while starting cocurrent when being warming up to 85 DEG C；First adduction flowing water glass then adds between sulfuric acid, control ph 9.5 ~ 10.5 at 9 ~ 10 to pH value；Cocurrent does not stop stirring after terminating, be acidified after adding sulfuric acid and dilution water progress, between terminal point control pH value 4.8 5.3；Ageing stirring reaction in 20 minutes terminates.The characteristics of there is Gao Bibiao, high oil absorption by silica made from the preparation method, and burning decrement is low, pH value is high, the cure time of rubber is shortened more than 50%, greatly improves processing efficiency.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of preparation side of rubber high reinforcing silica of high oil absorption
Method.
Background technology
Precipitated silica is commonly called as white carbon, also known as silicate hydrate, light silicon dioxide, and chemical expression can be written generally as
MSiO2nH2O, outward appearance is amorphous powder, the microballon of white high degree of dispersion.Precipitated silica is widely used in rubber system
All multirows such as product, tire, feed addictive, food additives, paint delustering agent, papermaking, silicon rubber, toothpaste abrasives, ink
Industry.
Silica is used in rubber applications as excellent reinforcing agent and filler, can greatly improve the physics of sizing material
Performance, reduces sizing material delayed.Silica can reduce tire drag in tire industry, while it is anti-slippery not lose its
Property, silica-filled sizing material is compared with the sizing material that ordinary carbon black is filled, and rolling resistance can reduce by 30%.
But it is single in terms of the reinforcing rubber effect for, the reinforcement ability of silica needs raising badly.
The content of the invention
The present invention is intended to provide a kind of preparation method of the rubber silica with high reinforcing property.
The preparation method of the high reinforcing silica of rubber high oil absorption comprises the following steps：
S1, accurate formulation concentration of sodium silicate is to 0.995 ~ 1.005 mol/l in make-up tank, and temperature control is in 25 ~ 50 DEG C of degree；
S2, the skill hot water 30m3 that changes a job from warm water tank, the glass 3.5m3 that adds water from refinery pit enter reactor, 60 DEG C are warming up to, by bottom liquid
Concentration is adjusted between 0.100 ~ 0.105 mol/l；
S3, step acidifying：While toward addition sulfuric acid and dilution water in reactor while stirring, pH is controlled between 6.5 ~ 7.0
After stop stirring and be aged 30 minutes；
S4, start stirring, while starting cocurrent when being warming up to 85 DEG C；First adduction flowing water glass then adds sulphur at 9 ~ 10 to pH value
Between acid, control ph 9.5 ~ 10.5；
S5, rear acidifying：Cocurrent does not stop stirring after terminating, be acidified after adding sulfuric acid and dilution water progress, terminal point control pH value 4.8-
5.3 between；
S6, ageing stirring reaction in 20 minutes terminate.
Further, first reactor is cleaned before step S2, makes it without wall dirt.
Preferably, step S3 is into step S5, and sour flow rate is 0.50 m3/h, and dilution water flow rate is 3.5 m3/h.
Preferably, in step S4, waterglass flow rate is 12.6 m3/h, stirring and 50 minutes cocurrent used times.
In step S3, jelly must occur after stopping stirring.
In step S4, the heating-up time is controlled at 30 minutes or so.
Preferably, concentration >=98% of sulfuric acid.
Pass through dioxide-containing silica made from the preparation method（w%） ≥ 98.5%；Burning decrement（w%）For 3.2 ~ 4.2；
Specific surface area（BET）(m2/g) it is 230 ~ 260；Loss on drying（w%）For 5.0 ~ 7.0；Oil factor（DBP absorption values)（ml/g）For
3.2~3.8；The characteristics of having Gao Bibiao, high oil absorption because of it, makes it have in rubber high reinforcing, and other physical property are also
Do not reduce；Meanwhile, the characteristics of its burning decrement is low, pH value is high make its apply rubber or tire cure time shorten 50% with
On, it is greatly improved processing efficiency.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, further is made to embodiment of the present invention below
It is described in detail on ground.
The present invention provides a kind of preparation method of the high reinforcing silica of rubber high oil absorption and comprised the following steps：
S1, accurate formulation concentration of sodium silicate is to 0.995 ~ 1.005 mol/l in make-up tank, and temperature control is in 25 ~ 50 DEG C of degree；
S2, the skill hot water 30m3 that changes a job from warm water tank, the glass 3.5m3 that adds water from refinery pit enter reactor, 60 DEG C are warming up to, by bottom liquid
Concentration is adjusted between 0.100 ~ 0.105 mol/l；
S3, step acidifying：While toward addition sulfuric acid and dilution water in reactor while stirring, sour flow rate is 0.50 m3/h, dilution
Rate of flow of water is 3.5 m3/h, by pH controls between 6.5 ~ 7.0 after stop stirring and be aged 30 minutes, glue must occur after stopping stirring
Freeze；
S4, start stirring, while start cocurrent when being warming up to 85 DEG C, the heating-up time is controlled at 30 minutes or so；First adduction flowing water
Glass, flow rate is 12.6 m3/h, then adds sulfuric acid at 9 ~ 10 to pH value, and sour flow rate is 0.50 m3/h, and cocurrent waterglass is total
Measure as 10.0m3, between control ph 9.5 ~ 10.5；
S5, rear acidifying：Cocurrent does not stop stirring after terminating, be acidified after adding sulfuric acid and dilution water progress, sour flow rate is 0.50 m3/
H, dilution water flow rate is between 3.5 m3/h, terminal point control pH value 4.8-5.3；
S6, ageing stirring reaction in 20 minutes terminate.
First reactor is cleaned before step S2, makes it without wall dirt.
In step S4, waterglass is stirred and 50 minutes cocurrent used times.
In the preparation method, concentration >=98% of sulfuric acid.
Pass through dioxide-containing silica made from the preparation method（w%） ≥ 98.5%；Burning decrement（w%）For 3.2 ~ 4.2；
Specific surface area（BET）(m2/g) it is 230 ~ 260；Loss on drying（w%）For 5.0 ~ 7.0；Oil factor（DBP absorption values)（ml/g）For
3.2~3.8；The characteristics of having Gao Bibiao, high oil absorption because of it, makes it have in rubber high reinforcing, and other physical property are also
Do not reduce；Meanwhile, the characteristics of its burning decrement is low, pH value is high make its apply rubber or tire cure time shorten 50% with
On, it is greatly improved processing efficiency.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (7)
1. a kind of rubber preparation method of the high reinforcing silica of high oil absorption, it is characterised in that comprise the following steps:
S1, accurate formulation concentration of sodium silicate is to 0.995 ~ 1.005 mol/l in make-up tank, and temperature control is in 25 ~ 50 DEG C of degree；
S2, the skill hot water 30m3 that changes a job from warm water tank, the glass 3.5m3 that adds water from refinery pit enter reactor, 60 DEG C are warming up to, by bottom liquid
Concentration is adjusted between 0.100 ~ 0.105 mol/l；
S3, step acidifying：While toward addition sulfuric acid and dilution water in reactor while stirring, pH is controlled between 6.5 ~ 7.0
After stop stirring and be aged 30 minutes；
S4, start stirring, while starting cocurrent when being warming up to 85 DEG C；First adduction flowing water glass then adds sulphur at 9 ~ 10 to pH value
Between acid, control ph 9.5 ~ 10.5；
S5, rear acidifying：Cocurrent does not stop stirring after terminating, be acidified after adding sulfuric acid and dilution water progress, terminal point control pH value 4.8-
5.3 between；
S6, ageing stirring reaction in 20 minutes terminate.
2. a kind of preparation method of rubber high reinforcing silica of high oil absorption according to claim 1, its feature
It is, first reactor is cleaned before step S2, makes it without wall dirt.
3. a kind of preparation method of rubber high reinforcing silica of high oil absorption according to claim 1, its feature
It is, step S3 is into step S5, and sour flow rate is 0.50 m3/h, and dilution water flow rate is 3.5 m3/h.
4. a kind of preparation method of rubber high reinforcing silica of high oil absorption according to claim 1, its feature
It is, in step S4, waterglass flow rate is 12.6 m3/h, stirring and 50 minutes cocurrent used times.
5. a kind of preparation method of rubber high reinforcing silica of high oil absorption according to claim 1, its feature
It is in step S3, jelly must occur after stopping stirring.
6. a kind of preparation method of rubber high reinforcing silica of high oil absorption according to claim 1, its feature
It is, in step S4, the heating-up time is controlled at 30 minutes or so.
7. a kind of preparation method of rubber high reinforcing silica of high oil absorption according to claim 1, its feature
It is, concentration >=98% of sulfuric acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516559A (en) * | 2018-05-25 | 2018-09-11 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low viscosity high oil absorption value Silica Using for Toothpaste |
| CN110835110A (en) * | 2019-12-12 | 2020-02-25 | 通化双龙硅材料科技有限公司 | Preparation method of precipitated hydrated silicon dioxide |
| CN111039298A (en) * | 2020-01-13 | 2020-04-21 | 福建省三明正元化工有限公司 | Preparation method of high-dispersion silicon dioxide |
| CN111153411A (en) * | 2020-01-13 | 2020-05-15 | 福建省三明正元化工有限公司 | Preparation method of silicon dioxide with excellent physical application performance |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008136019A2 (en) * | 2007-05-03 | 2008-11-13 | Council Of Scientific & Industrial Research | A process for the preparation of finely divided precipitated silica |
| CN101597065A (en) * | 2009-07-28 | 2009-12-09 | 通化双龙化工股份有限公司 | PE dividing plate Preparative Method of White Carbon Black |
| CN101618876A (en) * | 2009-08-18 | 2010-01-06 | 通化双龙化工股份有限公司 | Method for preparing precipitated white carbon black with controllable specific surface area |
| CN106185956A (en) * | 2016-07-12 | 2016-12-07 | 通化双龙化工股份有限公司 | A kind of preparation method of toothpaste precipitated silica thickening agent |
| CN106185957A (en) * | 2016-07-20 | 2016-12-07 | 福建远翔新材料股份有限公司 | The preparation method of tire silica reinforcing agent |
-
2017
- 2017-04-27 CN CN201710287776.XA patent/CN107021495A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008136019A2 (en) * | 2007-05-03 | 2008-11-13 | Council Of Scientific & Industrial Research | A process for the preparation of finely divided precipitated silica |
| CN101597065A (en) * | 2009-07-28 | 2009-12-09 | 通化双龙化工股份有限公司 | PE dividing plate Preparative Method of White Carbon Black |
| CN101618876A (en) * | 2009-08-18 | 2010-01-06 | 通化双龙化工股份有限公司 | Method for preparing precipitated white carbon black with controllable specific surface area |
| CN106185956A (en) * | 2016-07-12 | 2016-12-07 | 通化双龙化工股份有限公司 | A kind of preparation method of toothpaste precipitated silica thickening agent |
| CN106185957A (en) * | 2016-07-20 | 2016-12-07 | 福建远翔新材料股份有限公司 | The preparation method of tire silica reinforcing agent |
Non-Patent Citations (2)
| Title |
|---|
| 全国部分高校铸造专业《铸造化学》编写组: "《铸造化学》", 31 December 1976 * |
| 本书编委: "《辞海 数学物理化学分册》", 31 December 1987, 上海辞书出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516559A (en) * | 2018-05-25 | 2018-09-11 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low viscosity high oil absorption value Silica Using for Toothpaste |
| CN110835110A (en) * | 2019-12-12 | 2020-02-25 | 通化双龙硅材料科技有限公司 | Preparation method of precipitated hydrated silicon dioxide |
| CN111039298A (en) * | 2020-01-13 | 2020-04-21 | 福建省三明正元化工有限公司 | Preparation method of high-dispersion silicon dioxide |
| CN111153411A (en) * | 2020-01-13 | 2020-05-15 | 福建省三明正元化工有限公司 | Preparation method of silicon dioxide with excellent physical application performance |
| CN111153411B (en) * | 2020-01-13 | 2023-10-24 | 福建省三明正元化工有限公司 | Preparation method of silicon dioxide |
| CN111039298B (en) * | 2020-01-13 | 2023-10-24 | 福建省三明正元化工有限公司 | Preparation method of high-dispersion silicon dioxide |
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Application publication date: 20170808 |