CN106220914A - A kind of butadiene rubber liquid antioxidant and preparation method thereof - Google Patents
A kind of butadiene rubber liquid antioxidant and preparation method thereof Download PDFInfo
- Publication number
- CN106220914A CN106220914A CN201610658808.8A CN201610658808A CN106220914A CN 106220914 A CN106220914 A CN 106220914A CN 201610658808 A CN201610658808 A CN 201610658808A CN 106220914 A CN106220914 A CN 106220914A
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- CN
- China
- Prior art keywords
- butadiene rubber
- rubber liquid
- liquid antioxidant
- still
- antioxidant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a kind of butadiene rubber liquid antioxidant, it is characterised in that include following components in percentage by weight: phenol 45 ~ 55%, organic synthesis solvent 30 ~ 40%；Solid polymer 5 ~ 15% and catalyst 2 ~ 5%.Meanwhile, the invention also discloses the preparation method of butadiene rubber liquid antioxidant.The present invention has high oxidation resistance；Resistance to extractable is good, water insoluble and oily in；Good processability, non-volatile under the processing temperature of high polymer, do not decompose；Save input cost.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of butadiene rubber liquid antioxidant and preparation method thereof.
Background technology
Along with world wide class synthetic material, the especially yield of general plastic quickly increase, promote and have stimulated complete
Increasing rapidly of ball antioxidant production capacity, the production capacity of plastic antioxidants by the 130000 of nineteen ninety-five tons rise to 2003 240,000
More than Dun, it is maintained at about 8% with average growth rate per annum subsequently.The research direction of antioxidant has shifted towards helping of exploitation high-efficiency multi-function
Agent product and response type antioxidant, make full use of the synergism of antioxidant.
Summary of the invention
Goal of the invention: present invention aims to the deficiencies in the prior art, it is provided that a kind of butadiene rubber liquid antioxygen
Agent.
Another object of the present invention is to provide the preparation method of above-mentioned butadiene rubber liquid antioxidant.
Technical scheme: in order to reach foregoing invention purpose, the present invention is specifically achieved like this: a kind of butadiene rubber liquid
Body antioxidant, including following components in percentage by weight: phenol 45 ~ 55%, organic synthesis solvent 30 ~ 40%；Solid polymer 5
~ 15% and catalyst 2 ~ 5%.
Wherein, described phenol is 2,4-DTBP.
Wherein, described organic synthesis solvent is tert-dodecyl mercaptan.
Wherein, described solid polymer is paraformaldehyde.
Wherein, described catalyst is Dodecyl Dimethyl Amine.
The preparation method of a kind of butadiene rubber liquid antioxidant, comprises the following steps:
(1) under room temperature by the raw material evacuation feeding of the percentage by weight of formula ratio to reactor, be first evacuated in still
0.09mpa rushes nitrogen again to 0.05mpa, and continuous nitrogen is vented to normal pressure, still at N after replacing three times2It is warming up to 80 under protection
Closing steam valve after DEG C, be then to slowly warm up to 130 DEG C of insulation 0.5h, be further continued for being warmed up to 150 DEG C of insulation 2h, reaction terminates；Instead
Observing aqueous condition sample analysis during Ying, after analyzing, reactant purity reaches 85 ~ 90%, stops this step；
(2) it is cooled to 100 DEG C of washing stratification, adds in the phosphoric acid of reactant gross mass 20% and 40 ~ 50min, then wash quiet
Putting layering, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up, and temperature is raised to 150 DEG C and stops heating up, and keeps vacuum
It is cooled to 80 DEG C after state 3h, proceeds to finished product storage tank through filter and the most i.e. obtain butadiene rubber liquid antioxidant.
Beneficial effect: the present invention, compared with conventional art, has the advantage that
(1) there is high oxidation resistance；
(2) resistance to extractable is good, water insoluble and oily in；
(3) good processability, non-volatile under the processing temperature of high polymer, do not decompose；
(4) input cost has been saved.
Detailed description of the invention
Embodiment 1:
The phenol that percentage by weight is 50%, the organic synthesis solvent of 30% is taken under room temperature；The solid polymer of 15% and 5% urge
Agent evacuation feeding, to reactor, is first evacuated to 0.09mpa and rushes nitrogen again to 0.05mpa in still, continuous nitrogen displacement three
After secondary, emptying is to normal pressure, and still is interior at N2Close steam valve after being warming up to 80 DEG C under protection, be then to slowly warm up to 130 DEG C of insulations
0.5h, is further continued for being warmed up to 150 DEG C of insulation 2h, and reaction terminates；It is cooled to 100 DEG C of washing stratification, adds reactant gross mass
With 40 ~ 50min in the phosphoric acid of 20%, then washing stratification, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up,
Temperature is raised to 150 DEG C and stops heating up, and is cooled to 80 DEG C after keeping vacuum state 3h, proceeds to finished product storage tank inspection through filter qualified
After i.e. obtain butadiene rubber liquid antioxidant.
Embodiment 2:
The phenol that percentage by weight is 45%, the organic synthesis solvent of 40% is taken under room temperature；The solid polymer of 10% and 5% urge
Agent evacuation feeding, to reactor, is first evacuated to 0.09mpa and rushes nitrogen again to 0.05mpa in still, continuous nitrogen displacement three
After secondary, emptying is to normal pressure, and still is interior at N2Close steam valve after being warming up to 80 DEG C under protection, be then to slowly warm up to 130 DEG C of insulations
0.5h, is further continued for being warmed up to 150 DEG C of insulation 2h, and reaction terminates；It is cooled to 100 DEG C of washing stratification, adds reactant gross mass
With 40 ~ 50min in the phosphoric acid of 20%, then washing stratification, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up,
Temperature is raised to 150 DEG C and stops heating up, and is cooled to 80 DEG C after keeping vacuum state 3h, proceeds to finished product storage tank inspection through filter qualified
After i.e. obtain butadiene rubber liquid antioxidant.
Embodiment 3:
The phenol that percentage by weight is 55%, the organic synthesis solvent of 30% is taken under room temperature；The solid polymer of 12% and 3% urge
Agent evacuation feeding, to reactor, is first evacuated to 0.09mpa and rushes nitrogen again to 0.05mpa in still, continuous nitrogen displacement three
After secondary, emptying is to normal pressure, and still is interior at N2Close steam valve after being warming up to 80 DEG C under protection, be then to slowly warm up to 130 DEG C of insulations
0.5h, is further continued for being warmed up to 150 DEG C of insulation 2h, and reaction terminates；It is cooled to 100 DEG C of washing stratification, adds reactant gross mass
With 40 ~ 50min in the phosphoric acid of 20%, then washing stratification, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up,
Temperature is raised to 150 DEG C and stops heating up, and is cooled to 80 DEG C after keeping vacuum state 3h, proceeds to finished product storage tank inspection through filter qualified
After i.e. obtain butadiene rubber liquid antioxidant.
Embodiment 4:
The phenol that percentage by weight is 50%, the organic synthesis solvent of 40% is taken under room temperature；The solid polymer of 5% and 5% urge
Agent evacuation feeding, to reactor, is first evacuated to 0.09mpa and rushes nitrogen again to 0.05mpa in still, continuous nitrogen displacement three
After secondary, emptying is to normal pressure, and still is interior at N2Close steam valve after being warming up to 80 DEG C under protection, be then to slowly warm up to 130 DEG C of insulations
0.5h, is further continued for being warmed up to 150 DEG C of insulation 2h, and reaction terminates；It is cooled to 100 DEG C of washing stratification, adds reactant gross mass
With 40 ~ 50min in the phosphoric acid of 20%, then washing stratification, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up,
Temperature is raised to 150 DEG C and stops heating up, and is cooled to 80 DEG C after keeping vacuum state 3h, proceeds to finished product storage tank inspection through filter qualified
After i.e. obtain butadiene rubber liquid antioxidant.
Embodiment 5:
The phenol that percentage by weight is 55%, the organic synthesis solvent of 35% is taken under room temperature；The solid polymer of 8% and the catalysis of 2%
Agent evacuation feeding, to reactor, is first evacuated to 0.09mpa and rushes nitrogen again to 0.05mpa in still, continuous nitrogen is replaced three times
Rear emptying is to normal pressure, and still is interior at N2Close steam valve after being warming up to 80 DEG C under protection, be then to slowly warm up to 130 DEG C of insulation 0.5h,
Being further continued for being warmed up to 150 DEG C of insulation 2h, reaction terminates；It is cooled to 100 DEG C of washing stratification, adds reactant gross mass 20%
With 40 ~ 50min in phosphoric acid, then washing stratification, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up, temperature
Being raised to 150 DEG C stop heating up, be cooled to 80 DEG C after keeping vacuum state 3h, proceeding to finished product storage tank through filter is after the assay was approved
Obtain butadiene rubber liquid antioxidant.
Claims (6)
1. a butadiene rubber liquid antioxidant, it is characterised in that include following components in percentage by weight: phenol 45 ~ 55%,
Organic synthesis solvent 30 ~ 40%；Solid polymer 5 ~ 15% and catalyst 2 ~ 5%.
Butadiene rubber liquid antioxidant the most according to claim 1, it is characterised in that described phenol is 2,4-di-t-butyl
Phenol.
Butadiene rubber liquid antioxidant the most according to claim 1, it is characterised in that described organic synthesis solvent is uncle ten
Two carbon mercaptan.
Butadiene rubber liquid antioxidant the most according to claim 1, it is characterised in that described solid polymer is poly first
Aldehyde.
Butadiene rubber liquid antioxidant the most according to claim 1, it is characterised in that described catalyst is dodecyl two
Methyl tertiary amine.
6. the preparation method of a butadiene rubber liquid antioxidant, it is characterised in that comprise the following steps:
(1) under room temperature by the raw material evacuation feeding of the percentage by weight of formula ratio to reactor, be first evacuated in still
0.09mpa rushes nitrogen again to 0.05mpa, and continuous nitrogen is vented to normal pressure, still at N after replacing three times2It is warming up to 80 under protection
Closing steam valve after DEG C, be then to slowly warm up to 130 DEG C of insulation 0.5h, be further continued for being warmed up to 150 DEG C of insulation 2h, reaction terminates；Instead
Observing aqueous condition sample analysis during Ying, after analyzing, reactant purity reaches 85 ~ 90%, stops this step；
(2) it is cooled to 100 DEG C of washing stratification, adds in the phosphoric acid of reactant gross mass 20% and 40 ~ 50min, then wash quiet
Putting layering, still temperature evacuation when 100 DEG C takes off surplus moisture and gradually heats up, and temperature is raised to 150 DEG C and stops heating up, and keeps vacuum
It is cooled to 80 DEG C after state 3h, proceeds to finished product storage tank through filter and the most i.e. obtain butadiene rubber liquid antioxidant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610658808.8A CN106220914A (en) | 2016-08-12 | 2016-08-12 | A kind of butadiene rubber liquid antioxidant and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610658808.8A CN106220914A (en) | 2016-08-12 | 2016-08-12 | A kind of butadiene rubber liquid antioxidant and preparation method thereof |
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|---|---|
| CN106220914A true CN106220914A (en) | 2016-12-14 |
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| CN201610658808.8A Pending CN106220914A (en) | 2016-08-12 | 2016-08-12 | A kind of butadiene rubber liquid antioxidant and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7528285B2 (en) * | 2006-09-29 | 2009-05-05 | Korea Kumho Petrochemical Co., Ltd. | Method for preparing thiomethylphenols |
| CN103304716A (en) * | 2013-06-07 | 2013-09-18 | 常州大学 | Method for preparing liquid butadiene rubber anti-aging agent |
| CN104761478A (en) * | 2014-06-27 | 2015-07-08 | 江苏佳华新材料科技有限公司 | Preparation method of antioxidant 2,4-(dioctanethiol-6-methyl) phenol |
-
2016
- 2016-08-12 CN CN201610658808.8A patent/CN106220914A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7528285B2 (en) * | 2006-09-29 | 2009-05-05 | Korea Kumho Petrochemical Co., Ltd. | Method for preparing thiomethylphenols |
| CN103304716A (en) * | 2013-06-07 | 2013-09-18 | 常州大学 | Method for preparing liquid butadiene rubber anti-aging agent |
| CN104761478A (en) * | 2014-06-27 | 2015-07-08 | 江苏佳华新材料科技有限公司 | Preparation method of antioxidant 2,4-(dioctanethiol-6-methyl) phenol |
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Application publication date: 20161214 |
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