CN106751061A - The preparation method of brombutyl vulcanizate - Google Patents
The preparation method of brombutyl vulcanizate Download PDFInfo
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- CN106751061A CN106751061A CN201611083046.XA CN201611083046A CN106751061A CN 106751061 A CN106751061 A CN 106751061A CN 201611083046 A CN201611083046 A CN 201611083046A CN 106751061 A CN106751061 A CN 106751061A
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- biir
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- vulcanizate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
- C08F8/22—Halogenation by reaction with free halogens
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
- C08L23/283—Halogenated homo- or copolymers of iso-olefins
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of brombutyl vulcanizate.The preparation method of brombutyl vulcanizate, comprises the following steps：（1）The preparation of BIIR；（2）The preparation of BIIR vulcanizates.The brombutyl vulcanizate that the present invention is made its tensile strength, elongation at break and shore a hardness it is higher.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of brombutyl vulcanizate.
Background technology
Brombutyl (BIIR) is the brominated product of isobutene and isoprene copolymer, i.e., in butyl rubber
(IIR) bromine atoms are introduced in strand.After IIR brominations in addition to extra crosslinking sites are produced, while increased the anti-of double bond
Should activity.BIIR in addition to the characteristic with IIR, also with rate of cure it is fast and other rubber compatibilities are good, mutual viscosity improves,
The features such as individually being vulcanized and be had more preferable heat resistance with zinc oxide, thus be that manufacture tubeless tyre and pharmaceutical products can not
The raw material of replacement.At present, the production method of BIIR mainly has dry glue to knead and 2 kinds of solution bromination method.Dry glue kneads method because not anti-
The bromating agent and its byproduct answered are not removed and remained in rubber, influence the performance of sizing material, unstable product quality.Solution bromine
, because reaction is uniform and steady quality, operating procedure is simple, and properties of product are excellent, thus the head being modified as IIR brominations for change method
Choosing method.Compared with BIIR is prepared from IIR slurry, the direct bromination synthesis BIIR of IIR glues prepared by solwution method, it is to avoid
The dissolution process of solvent switching or sizing material needed for the former；Additionally, the latter prepares BIIR uses mixed solvent, toxicity is smaller,
Environmental pollution is lighter, and the corrosivity to equipment is smaller.Because existing slurry process prepares the solution brominations of IIR mono- production BIIR works
Skill reaction rate is slower, and prolonging for fully reaction, raising bromine utilization rate, but residence time can only be realized by the extension reaction time
Length can cause addition reaction largely to occur.
The content of the invention
The present invention is directed to propose a kind of preparation method of brombutyl vulcanizate.
Technical program of the present invention lies in：
The preparation method of brombutyl vulcanizate, comprises the following steps：
（1）The preparation of BIIR
350 mL IIR glues are added in 1 L bromination reaction kettles, 150 mL cosolvent CH are added2C12With 30 mL mass point
Number is 5% oxidant NaClO solution, is then heated to 40 DEG C, and bromine is diluted in hexane solution, is configured to mass fraction
It is the hexane solution of 2l%, is rapidly added under normal pressure, lucifuge and constant temperature in above-mentioned glue mixed solution, in high-speed stirred
2.5 min of lower reaction；After reaction terminates, in adding 35 mL mass fractions to be 7% NaOH solution reactant, 20 are neutralized
Stop stirring after min, it is 7 that glue is washed with distilled water to pH value, adds antioxidant 1330, calcium stearate and deacidification agent
ESBO, is eventually adding boiling water and flashes off solvent, and the blocking precipitation of rubber reunion after dehydration, being vacuum dried, is opened at 100 ~ 120 DEG C
The min of mill 2 ~ 5 in mill, removes residual moisture, stand-by；
（2）The preparation of BIIR vulcanizates
Formula：BIIR 80 ~ 100, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2, DBP 2 promote
Enter agent DM 1.5, anti-aging agent RD 1.5；
BIIR is plasticated in being placed in mill after 60 DEG C of h of constant temperature 12, above-mentioned various compounding aids are then sequentially added, kneaded
Uniformly, thin logical bottom sheet；After elastomeric compound parks 22 ~ 24 h, vulcanized on vulcanizing press, be made BIIR vulcanizates.
Described conditions of vulcanization is 160 DEG C × 10 min.
Described formula be BIIR 80, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2,
DBP 2, altax 1.5, anti-aging agent RD 1.5.
Described formula be BIIR 92, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2,
DBP 2, altax 1.5, anti-aging agent RD 1.5.
The technical effects of the invention are that：
The brombutyl vulcanizate that the present invention is made its tensile strength, elongation at break and shore a hardness it is higher.
Specific embodiment
The preparation method of brombutyl vulcanizate, comprises the following steps：
Embodiment 1
（1）The preparation of BIIR
350 mL IIR glues are added in 1 L bromination reaction kettles, 150 mL cosolvent CH are added2C12With 30 mL mass point
Number is 5% oxidant NaClO solution, is then heated to 40 DEG C, and bromine is diluted in hexane solution, is configured to mass fraction
It is the hexane solution of 2l%, is rapidly added under normal pressure, lucifuge and constant temperature in above-mentioned glue mixed solution, in high-speed stirred
2.5 min of lower reaction；After reaction terminates, in adding 35 mL mass fractions to be 7% NaOH solution reactant, 20 are neutralized
Stop stirring after min, it is 7 that glue is washed with distilled water to pH value, adds antioxidant 1330, calcium stearate and deacidification agent
ESBO, is eventually adding boiling water and flashes off solvent, and the blocking precipitation of rubber reunion after dehydration, being vacuum dried, is opened at 100 ~ 120 DEG C
The min of mill 2 ~ 5 in mill, removes residual moisture, stand-by；
（2）The preparation of BIIR vulcanizates
Formula：BIIR 80 ~ 100, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2, DBP 2 promote
Enter agent DM 1.5, anti-aging agent RD 1.5；
BIIR is plasticated in being placed in mill after 60 DEG C of h of constant temperature 12, above-mentioned various compounding aids are then sequentially added, kneaded
Uniformly, thin logical bottom sheet；After elastomeric compound parks 22 ~ 24 h, vulcanized on vulcanizing press, be made BIIR vulcanizates.Wherein,
Described conditions of vulcanization is 160 DEG C × 10 min.
Embodiment 2
（1）The preparation of BIIR
350 mL IIR glues are added in 1 L bromination reaction kettles, 150 mL cosolvent CH are added2C12With 30 mL mass point
Number is 5% oxidant NaClO solution, is then heated to 40 DEG C, and bromine is diluted in hexane solution, is configured to mass fraction
It is the hexane solution of 2l%, is rapidly added under normal pressure, lucifuge and constant temperature in above-mentioned glue mixed solution, in high-speed stirred
2.5 min of lower reaction；After reaction terminates, in adding 35 mL mass fractions to be 7% NaOH solution reactant, 20 are neutralized
Stop stirring after min, it is 7 that glue is washed with distilled water to pH value, adds antioxidant 1330, calcium stearate and deacidification agent
ESBO, is eventually adding boiling water and flashes off solvent, and the blocking precipitation of rubber reunion after dehydration, being vacuum dried, is opened at 100 ~ 120 DEG C
The min of mill 2 ~ 5 in mill, removes residual moisture, stand-by；
（2）The preparation of BIIR vulcanizates
Formula：BIIR 80, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2, DBP 2, accelerator
DM 1.5, anti-aging agent RD 1.5；
BIIR is plasticated in being placed in mill after 60 DEG C of h of constant temperature 12, above-mentioned various compounding aids are then sequentially added, kneaded
Uniformly, thin logical bottom sheet；After elastomeric compound parks 22 ~ 24 h, vulcanized on vulcanizing press, be made BIIR vulcanizates.Wherein,
Described conditions of vulcanization is 160 DEG C × 10 min.
Claims (4)
1. the preparation method of brombutyl vulcanizate, it is characterised in that comprise the following steps：
（1）The preparation of BIIR
350 mL IIR glues are added in 1 L bromination reaction kettles, 150 mL cosolvent CH are added2C12With 30 mL mass point
Number is 5% oxidant NaClO solution, is then heated to 40 DEG C, and bromine is diluted in hexane solution, is configured to mass fraction
It is the hexane solution of 2l%, is rapidly added under normal pressure, lucifuge and constant temperature in above-mentioned glue mixed solution, in high-speed stirred
2.5 min of lower reaction；After reaction terminates, in adding 35 mL mass fractions to be 7% NaOH solution reactant, 20 are neutralized
Stop stirring after min, it is 7 that glue is washed with distilled water to pH value, adds antioxidant 1330, calcium stearate and deacidification agent
ESBO, is eventually adding boiling water and flashes off solvent, and the blocking precipitation of rubber reunion after dehydration, being vacuum dried, is opened at 100 ~ 120 DEG C
The min of mill 2 ~ 5 in mill, removes residual moisture, stand-by；
（2）The preparation of BIIR vulcanizates
Formula：BIIR 80 ~ 100, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2, DBP 2 promote
Enter agent DM 1.5, anti-aging agent RD 1.5；
BIIR is plasticated in being placed in mill after 60 DEG C of h of constant temperature 12, above-mentioned various compounding aids are then sequentially added, kneaded
Uniformly, thin logical bottom sheet；After elastomeric compound parks 22 ~ 24 h, vulcanized on vulcanizing press, be made BIIR vulcanizates.
2. the preparation method of brombutyl vulcanizate according to claim 1, it is characterised in that：Described vulcanization bar
Part is 160 DEG C × 10 min.
3. the preparation method of brombutyl vulcanizate according to claim 1, it is characterised in that：Described formula is
BIIR 80, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2, DBP 2, altax 1.5 is prevented
Old agent RD 1.5.
4. the preparation method of brombutyl vulcanizate according to claim 1, it is characterised in that：Described formula is
BIIR 92, N 660 60, magnesia 5, stearic acid 1, zinc oxide 5, paraffin oil 5, DOP 2, DBP 2, altax 1.5 is prevented
Old agent RD 1.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611083046.XA CN106751061A (en) | 2016-11-30 | 2016-11-30 | The preparation method of brombutyl vulcanizate |
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| CN201611083046.XA CN106751061A (en) | 2016-11-30 | 2016-11-30 | The preparation method of brombutyl vulcanizate |
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| CN201611083046.XA Pending CN106751061A (en) | 2016-11-30 | 2016-11-30 | The preparation method of brombutyl vulcanizate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244575A (en) * | 2018-08-15 | 2019-01-18 | 宁德三行技研工贸有限公司 | The sucker and its processing method vacuumized for rectangular plastic housing formation of Li-ion batteries |
-
2016
- 2016-11-30 CN CN201611083046.XA patent/CN106751061A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244575A (en) * | 2018-08-15 | 2019-01-18 | 宁德三行技研工贸有限公司 | The sucker and its processing method vacuumized for rectangular plastic housing formation of Li-ion batteries |
| CN109244575B (en) * | 2018-08-15 | 2020-05-19 | 宁德三行技研工贸有限公司 | Sucking disc for formation and vacuum pumping of square molded case lithium battery and processing method thereof |
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Application publication date: 20170531 |