CN102140190B - Rubber tire extending oil for improving low hysteretic loss of rubber tire and preparation method thereof - Google Patents
Rubber tire extending oil for improving low hysteretic loss of rubber tire and preparation method thereof Download PDFInfo
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- CN102140190B CN102140190B CN2010101048014A CN201010104801A CN102140190B CN 102140190 B CN102140190 B CN 102140190B CN 2010101048014 A CN2010101048014 A CN 2010101048014A CN 201010104801 A CN201010104801 A CN 201010104801A CN 102140190 B CN102140190 B CN 102140190B
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- rubber tire
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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
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses a rubber tire extending oil for improving low hysteretic loss of a rubber tire and a preparation method thereof. The rubber tire extending oil comprises raw materials by weight portion: 30 to 60 portions of saturated isoparaffin oil, 20 to 50 portions of LAL saturated hydrocarbon, 5 to 50 portions of cycloparaffin oil and 0 to 35 portion(s) of saturated aromatic oil; the preparation method comprises the following steps: all the raw materials are mixed together for crosslinking reaction so as to obtain a product with bromine value of below 15, and the extending oil is obtained by temperature reduction and material discharging. The rubber tire extending oil reaches the environmental protection requirements of European Union in environmental protection issues, has lowhysteretic loss and physical performances such as wide viscosity, colloidal property and the like. The rubber tire has very good low hysteretic loss characteristic and is used for tire production andcan effectively improve performance and quality of tires.
Description
Technical field
The present invention relates to a kind of rubber tire filling, relate in particular to a kind of rubber tire filling of improving the low hysteresis loss of rubber tyre and preparation method thereof, belong to the production field of rubber tyre.
Background technology
Just can not enter the European market from January 1st, 2010 if tire contains (the instruction 2005/69/EC) that do not meet EU Committee's issue, because the content of polycyclic aromatic hydrocarbons and polycyclc aromatic compound is higher, main products (being aromatic hydrocarbon oil (DAE)) as rubber for tire extending oil does not meet the requirement of new legislation traditionally, thereby need replace with the less substitute products of toxicity.
European Union and even the whole world propose to substitute aromatic hydrocarbon oil, and have proposed tire drag to be reduced by 50% 10 years futures, realize the low-carbon (LC) target.At present, tire formulation is badly in need of wanting a kind of low hysteresis loss environmental friendly material process oil.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provides a kind of toxicity little and can effectively improve the rubber tire filling of the low hysteresis loss of rubber tyre.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of rubber tire filling of improving the low hysteresis loss of rubber tyre comprises that each raw material of following weight part is made:
Saturation isomerism alkane oil 30-60 part, the saturated hydrocarbon ils 20-50 of LAL part, naphthenic oil 5-50 part, saturated aromatic hydrocarbon oil 0-35 part;
Preferably, the weight part of each raw material is: saturation isomerism alkane oil 40-60 part, the saturated hydrocarbon ils 20-30 of LAL part, naphthenic oil 8-12 part, saturated aromatic hydrocarbon oil 2-28 part;
Wherein, described saturation isomerism alkane oil is that isoparaffin is obtained by the processing of impurity elimination ring refinement treatment; Isoparaffin comes from refinery's vacuum distillate (2 34 lines reduce pressure), and isoparaffin consists of: the N-alkanes of straight chain accounts for 20%, and the isomeric alkane of side chain accounts for 80%.
Described impurity elimination ring refinement treatment working method comprises: refining: refilter clean with carclazyte absorption isoparaffin; Hydrotreatment: will make with extra care the back isoparaffin and carry out hydrotreatment, and describedly add hydrotreated condition optimization and be: in the presence of metallic nickel, 180-300 ℃ of temperature maintenance, pressure is the 0.8-1 MPa, the time is 10-20 hour.
The preparation method of the saturated hydrocarbon ils of described LAL comprises:
(1) takes by weighing each component by following weight part: vinylbenzene 40-45 part, indenes 10-25 part, cyclopentadiene 20-30 part, vinyl toluene 0-5 part, dication aluminum chloride 0.05-0.15 part, auxiliary 100-150 part; Wherein, described auxiliary can be toluene or dimethylbenzene;
(2) described each raw material of step (1) is mixed carry out dication catalysis low-temp reaction;
(3) with the resulting product standing demix of step (2), take off layer liquid and slough residual fraction, obtain body of paste;
(4) take by weighing each component by following weight: the resulting body of paste 40-50 of step (3) part, isoparaffin 35-45 part, aromatic hydrocarbon oil 10-20 part; To carry out the hydrogenation processing after the said components mixing, namely; Wherein, describedly add hydrogenation and handle and to comprise: in the presence of metallic nickel, temperature keeps 180-300 ℃, and pressure is the 0.8-1 MPa, adds hydrogenation processing 10-20 hour.
" isoparaffin " of the present invention comes from refinery's vacuum distillate (2 34 lines reduce pressure), and isoparaffin consists of: the N-alkanes of straight chain accounts for 20%, and the isomeric alkane of side chain accounts for 80%
Described " aromatic hydrocarbon oil " belongs to the polycyclic aromatic hydrocarbons mixture, total can satisfy requirement of the present invention as long as contain the aromatic hydrocarbons of 30-45wt% in its composition, this aromatic hydrocarbons mainly comprises cyclopentadiene-1.3. dicyclopentadiene, compositions such as vinyl toluene.
Described saturated aromatic hydrocarbon oil is aromatic hydrocarbon oil to be carried out the processing of impurity elimination ring and saturated refinement treatment obtain; Aromatic hydrocarbon oil is carried out the saturated processing of severe hydrogenation just obtain saturated aromatic hydrocarbon oil, it adds hydrotreated condition optimization: in the presence of metallic nickel, be 180-300 ℃ in temperature, pressure is to add hydrogenation under the condition of 0.8-1 MPa to handle, and the treatment time is preferably 10-20 hour.
Described naphthenic hydrocarbon can be that general formula is CnH
2The compound of the ring texture of n divides five carbocyclic rings and hydrogenation of six carbocyclic, and its main body is not carbochain but carbocyclic ring for example can be pentamethylene, hexanaphthene or dimethyl cyclohexane etc.
Preferably 200 ℃-360 ℃ of the boiling spreads of each raw material that the present invention uses.
Another technical problem to be solved by this invention provides a kind of above-mentioned method of improving the rubber tire filling of the low hysteresis loss of rubber tyre for preparing.
Another technical problem to be solved by this invention is achieved through the following technical solutions:
A kind ofly prepare the above-mentioned method of improving the rubber tire filling of the low hysteresis loss of rubber tyre, comprising:
(1) takes by weighing each raw material by described weight part;
(2) each raw material is mixed after, carry out crosslinkedization reaction, obtain bromine number 15 with interior product, the cooling discharge, namely.
Wherein, described crosslinkedization reaction is preferably carried out crosslinkedization reaction under temperature is 50-400 ℃ condition; Preferred, described crosslinkedization reaction is carried out under the following conditions: at temperature 220-300 ℃, pressure is to stir 2-5 hour under the condition of 1.5-2 MPa; Wherein, when stirring, constantly charge into CO
2Shielding gas (CO
2Add-on is preferably and per hour adds 2 kilograms of CO
2Gas).
Rubber tire filling of the present invention reaches the European Union environmental protection requirement in environmental protection, have low hysteresis loss characteristic and viscosity, close colloidality and other physicals widely, rubber tire filling of the present invention is for the production of tire, have well low hysteresis loss characteristic, can effectively improve performance and the quality of tire.
Embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage of the present invention and characteristics will be more clear along with description.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.It will be understood by those skilled in the art that and down can make amendment or replace the details of technical solution of the present invention and form without departing from the spirit and scope of the present invention, but these modifications and replacing all fall within the scope of protection of the present invention.
One, the preparation of used each raw material of the present invention
1, the preparation of saturation isomerism alkane oil:
Raw material and source: isoparaffin, come from refinery's vacuum distillate (2 34 lines reduce pressure), isoparaffin consists of: the N-alkanes of straight chain accounts for 20%, and the isomeric alkane of side chain accounts for 80%.
Impurity elimination ring refinement treatment working method comprises: refining: refilter clean with carclazyte absorption isoparaffin; Hydrotreatment: will make with extra care the back isoparaffin and carry out hydrotreatment namely under the following conditions: in the presence of metallic nickel, temperature keeps 180-300 ℃, and pressure is the 0.8-1 MPa, handles 10-20 hour, namely.
2, the preparation of the saturated hydrocarbon ils of LAL:
1, takes by weighing each component by following weight: vinylbenzene cut 40kg, indenes cut 25kg, cyclopentadiene cut 30kg, vinyl toluene cut 5kg, dication aluminum chloride (available from resin institute of Qingdao Haijia Additives Co., Ltd., trade name " dication aluminum chloride ") 0.1kg;
2, above-mentioned each component is mixed after, be auxiliary with the toluene of 100kg, charging into CO
2Under the condition of gas shield, reaction is 30 hours under 15 ℃ of conditions of temperature;
3, the resulting product of step 2 is added methyl alcohol 2kg under 15 ℃ of conditions of temperature, 35 ℃ of constant temperature stirred 3 hours;
4, with refining layering under the resulting product normal temperature of step 3 12 hours, take off layer liquid and under 260 ℃ of temperature, slough residual fraction, obtain the thick liquid that flows 40-50 ℃ of temperature range.
5, take by weighing each component by following weight: the thick liquid 45kg that step 4 is prepared, isoparaffin 40kg, aromatic hydrocarbon oil 15kg; Above-mentioned each component mixed under 300 ℃ of conditions carry out hybrid reaction after 4 hours, add hydrogenation and handle: in the presence of metallic nickel, 180-300 ℃ of temperature maintenance, pressure is the 0.8-1 MPa, handles 10-20 hour, namely.
3, the preparation of saturated aromatic hydrocarbon oil:
Raw material: aromatic hydrocarbon oil belongs to the polycyclic aromatic hydrocarbons mixture, total as long as contain the aromatic hydrocarbons of 30-45wt% in its composition, wherein said aromatic hydrocarbons comprises cyclopentadiene-1.3. dicyclopentadiene, vinyl toluene etc.;
Aromatic hydrocarbon oil is carried out the saturated processing of severe hydrogenation just obtain saturated aromatic hydrocarbon oil, it adds hydrotreated condition and is: in the presence of metallic nickel, be 180-300 ℃ in temperature, pressure is to add hydrogenation under the condition of 0.8-1 MPa to handle, and the treatment time is 10-20 hour.
4, naphthenic oil: be that general formula is C
nH
2nRing texture, divide five carbocyclic rings and hydrogenation of six carbocyclic, its main body is not carbochain but carbocyclic ring, the main component that comprises has pentamethylene, hexanaphthene is or/and dimethyl cyclohexane etc.
Embodiment 1
Take by weighing each raw material (unit: kg): saturation isomerism alkane oil 40, the saturated hydrocarbon ils 20 of LAL, naphthenic oil 12, saturated aromatic hydrocarbon oil 28 by following weight;
Under 300 ℃ of temperature condition, stirred 5 hours under pressure 1.5 MPas.Constantly charge into CO during stirring
2Shielding gas is surveyed bromine number 15 with after interior, and the cooling discharge obtains to stablize saturated oil product.
Embodiment 2
Take by weighing each raw material (unit: kg): saturation isomerism alkane oil 60, the saturated hydrocarbon ils 30 of LAL, naphthenic oil 8, saturated aromatic hydrocarbon oil 2 by following weight;
Under 220 ℃ of temperature condition, stirred 2 hours under pressure 2 MPas.Constantly charge into CO during stirring
2Shielding gas.Survey bromine number 15 with after interior, the cooling discharge obtains to stablize saturated oil product.
Embodiment 3
Take by weighing each raw material (unit: kg): saturation isomerism alkane oil 30, the saturated hydrocarbon ils 20 of LAL, naphthenic oil 5 by following weight;
Under 280 ℃ of temperature condition, stirred 3 hours under pressure 1.8 MPas.Constantly charge into CO during stirring
2Shielding gas.Survey bromine number 15 with after interior, the cooling discharge obtains to stablize saturated oil product.
Embodiment 4
Take by weighing each raw material (unit: kg): saturation isomerism alkane oil 60, the saturated hydrocarbon ils 50 of LAL, naphthenic oil 50, saturated aromatic hydrocarbon oil 35 by following weight;
Under 250 ℃ of temperature condition, stirred 4 hours under pressure 2 MPas.Constantly charge into CO during stirring
2Shielding gas is surveyed bromine number 15 with after interior, and the cooling discharge obtains to stablize saturated oil product.
The environmental protection tests result of test example 1 rubber tire filling of the present invention
Detected object: the rubber tire filling that embodiment 1-4 is prepared;
Examination criteria: 2005/69/EC; Detect and require to see Table 1.
Table 1 detects requirement
| Parameter | Unit | Limit value |
| Benzo (a) pyrene | mg/kg | 1 |
| The polycyclic aromatic hydrocarbons sum | mg/kg | 10 |
Detection method and result: detection method: solvent extraction and quantitatively gaschromatographic mass spectrometry selectivity detection (GC-MS); Detected result sees Table 2.
Detected object has all passed through the environmental protection tests project that examination criteria sets; Illustrate that rubber tire filling of the present invention reaches the European Union environmental protection requirement in environmental protection.
Table 2
Annotate: " mg/kg " refers to every kilogram of milligram
" ND " refers to＜0.2mg/kg.
Test example 2 rubber tire filling of the present invention are used and physicals analysis (table 2) in the tire sidewall prescription
Supply test agent: the rubber tire filling that embodiment 1-4 is prepared;
Control sample: common aromatic hydrocarbon oil (available from the Shandong Jinan Refinery).
Test method: use and physicals in the tire sidewall prescription for test agent according to the described prescription test of table 2;
Test-results: see Table 3.
Table 2
Table 3 sizing compound formula performance inventory
Test example 3 rubber tire filling of the present invention are used and the physicals analysis in the tyre crown prescription
Supply test agent: the rubber tire filling that embodiment 1-4 is prepared;
Control sample 1: common aromatic hydrocarbon oil; (available from the Shandong Jinan Refinery)
Control sample 2: the holy 500TDAE environmental protection of Chinese oil; (moiety: aromatic hydrocarbon oil; Buy the source: the CHINESE REGION commission merchant of Han Sheng company)
Test method: use and physicals in the tyre crown prescription for test agent according to the described prescription test of table 4;
Test-results: see Table 5.
Table 4
| For test agent | ----- | 18.00 | ----- |
| The holy 500TDAE environmental protection of Chinese oil | ----- | ----- | 18.00 |
| Common SULPHUR POWDER | 2.20 | 2.20 | 2.20 |
| Accelerator NS | 1.10 | 1.10 | 1.10 |
| Amount to: | 227.3 | 227.3 | 227.3 |
Table 5 sizing compound formula performance inventory
Claims (13)
1. a rubber tire filling of improving the low hysteresis loss of rubber tyre comprises that each raw material of following weight part is made: saturation isomerism alkane oil 30-60 part, the saturated hydrocarbon ils 20-50 of LAL part, naphthenic oil 5-50 part and saturated aromatic hydrocarbon oil 0-35 part; The preparation method of the saturated hydrocarbon ils of described LAL comprises: (1) takes by weighing each raw material by following weight part: 40-45 parts of vinylbenzene, 10-25 parts of indenes, 20-30 parts of cyclopentadiene, 0-5 parts of vinyl toluenes, dication aluminum chloride 0.05-0.15 part, 100-150 parts of auxiliarys; (2) described raw material is mixed carry out dication catalysis low-temp reaction; (3) with the resulting product standing demix of step (2), take off layer liquid and slough residual fraction, obtain body of paste; (4) take by weighing each component by following weight: the resulting body of paste 40-50 of step (3) part, isoparaffin 35-45 part, aromatic hydrocarbon oil 10-20 part; To carry out the hydrogenation processing after the said components mixing, namely.
2. according to the described rubber tire filling of claim 1, it is characterized in that the weight part of each raw material is: saturation isomerism alkane oil 40-60 part, the saturated hydrocarbon ils 20-30 of LAL part, naphthenic oil 8-12 part, saturated aromatic hydrocarbon oil 2-28 part.
3. according to claim 1 or 2 described rubber tire filling, it is characterized in that the preparation method of described saturation isomerism alkane oil comprises: isoparaffin is carried out the severe hydrogenation, namely.
4. according to the described rubber tire filling of claim 3, it is characterized in that: the consisting of of described isoparaffin: the N-alkanes of straight chain accounts for 20%, and the isomeric alkane of side chain accounts for 80%; Described severe method of hydrotreating comprises: (1) is refining: refilter clean with carclazyte absorption isoparaffin; (2) hydrotreatment: will make with extra care the back isoparaffin and carry out hydrotreatment, hydrotreated condition is: in the presence of metallic nickel, temperature keeps 180-300 ℃, and pressure is the 0.8-1 MPa, and the hydrogen treatment time is 10-20 hour.
5. according to the described rubber tire filling of claim 1, it is characterized in that: described auxiliary comprises toluene or dimethylbenzene; Describedly add hydrogenation and handle and to comprise: in the presence of metallic nickel, 180-300 ℃ of temperature maintenance, pressure is the 0.8-1 MPa, adding the hydrogenation treatment time is 10-20 hour.
6. according to claim 1 or 2 described rubber tire filling, it is characterized in that described saturated aromatic hydrocarbon oil preparation method comprises: aromatic hydrocarbon oil is carried out the severe hydrogenation, namely.
7. according to the described rubber tire filling of claim 6, it is characterized in that: described aromatic hydrocarbon oil is the polycyclic aromatic hydrocarbons mixture, mainly contains the aromatic hydrocarbons of 30-45wt% in its total composition; Described severe method of hydrotreating comprises: in the presence of metallic nickel, be 180-300 ℃ in temperature, pressure is to add hydrogenation under the condition of 0.8-1 MPa to handle, and the hydrogen treatment time is 10-20 hour.
8. according to claim 1 or 2 described rubber tire filling, it is characterized in that: described naphthenic oil is that general formula is C
nH
2nRing texture, include five carbocyclic rings and hydrogenation of six carbocyclic, main body belongs to the carbocyclic ring structure.
9. according to the described rubber tire filling of claim 8, it is characterized in that: described naphthenic oil comprises: pentamethylene, hexanaphthene is or/and dimethyl cyclohexane.
10. method for preparing claim 1 or 2 described rubber tire filling comprises:
(1) takes by weighing each raw material by described weight part;
(2) each raw material is mixed after, carry out crosslinkedization reaction, obtain bromine number 15 with interior product, the cooling discharge, namely.
11. it is characterized in that in accordance with the method for claim 10: it is to carry out under 50-400 ℃ the condition that described crosslinkedization is reflected at temperature.
12. in accordance with the method for claim 11, it is characterized in that described crosslinkedization reaction comprises: be to stir 2-5 hour under the condition of 1.5-2 MPa at temperature 220-300 ℃, pressure; Wherein, when stirring, constantly charge into shielding gas CO
2
13. claim 1 or the 2 described rubber tire filling purposes in the preparation tire.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101048014A CN102140190B (en) | 2010-02-03 | 2010-02-03 | Rubber tire extending oil for improving low hysteretic loss of rubber tire and preparation method thereof |
| PCT/CN2010/072321 WO2011094973A1 (en) | 2010-02-03 | 2010-04-29 | Rubber tyre extender oil for improving low hysteresis loss of rubber tyre and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101048014A CN102140190B (en) | 2010-02-03 | 2010-02-03 | Rubber tire extending oil for improving low hysteretic loss of rubber tire and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102140190A CN102140190A (en) | 2011-08-03 |
| CN102140190B true CN102140190B (en) | 2013-10-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101048014A Active CN102140190B (en) | 2010-02-03 | 2010-02-03 | Rubber tire extending oil for improving low hysteretic loss of rubber tire and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN102140190B (en) |
| WO (1) | WO2011094973A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516704B (en) * | 2011-12-22 | 2013-06-12 | 宫相勤 | Waterproof material and its preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1976985A (en) * | 2004-06-03 | 2007-06-06 | 国际壳牌研究有限公司 | Process for the preparation of rubber extender oil compositions |
| CN101415807A (en) * | 2006-03-31 | 2009-04-22 | 新日本石油株式会社 | Polyfunctional hydrocarbon oil composition |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048505C (en) * | 1994-05-24 | 2000-01-19 | 青岛领丰化工有限公司 | Method for producing styrene indene resin |
| US5853569A (en) * | 1997-12-10 | 1998-12-29 | Exxon Research And Engineering Company | Method for manufacturing a process oil with improved solvency |
| US20080085970A1 (en) * | 2006-10-02 | 2008-04-10 | The Yokohama Rubber Co., Ltd. | Rubber composition for tire inner liner and pneumatic tire using the same |
-
2010
- 2010-02-03 CN CN2010101048014A patent/CN102140190B/en active Active
- 2010-04-29 WO PCT/CN2010/072321 patent/WO2011094973A1/en unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1976985A (en) * | 2004-06-03 | 2007-06-06 | 国际壳牌研究有限公司 | Process for the preparation of rubber extender oil compositions |
| CN101415807A (en) * | 2006-03-31 | 2009-04-22 | 新日本石油株式会社 | Polyfunctional hydrocarbon oil composition |
Non-Patent Citations (2)
| Title |
|---|
| 全氢法高压加氢工艺生产优质环烷基橡胶油产品;尹宏;《橡胶科技市场》;20041231(第4期);18-21 * |
| 尹宏.全氢法高压加氢工艺生产优质环烷基橡胶油产品.《橡胶科技市场》.2004,(第4期), |
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| Publication number | Publication date |
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| WO2011094973A1 (en) | 2011-08-11 |
| CN102140190A (en) | 2011-08-03 |
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