CN107236083A - Modified graphene nitrile rubber latex and its production technology - Google Patents
Modified graphene nitrile rubber latex and its production technology Download PDFInfo
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- CN107236083A CN107236083A CN201710423299.5A CN201710423299A CN107236083A CN 107236083 A CN107236083 A CN 107236083A CN 201710423299 A CN201710423299 A CN 201710423299A CN 107236083 A CN107236083 A CN 107236083A
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- butadiene
- tank
- acrylonitrile
- rubber latex
- kettle
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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
- C08F236/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F236/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F236/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F236/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated with nitriles
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The present invention provides a kind of modified graphene nitrile rubber latex and its production technology, belong to rubber latex chemical technology field, the modified graphene nitrile rubber latex is using butadiene and acrylonitrile as principal monomer, add graphene, using unsaturated carboxylic acid, and it is aided with many double bond type cross-linking monomers and/or other function monomers, carry out polymerisation and obtain product, composite emulsifying system is used during polymerization, that is reactive emulsifier and a small amount of anion emulsifier, persulfate is initiator, and alkyl hydrosulfide is molecular weight regulator, and other auxiliary agents, improve conversion ratio.The modified graphene nitrile rubber latex is the reaction polymer of the materials such as butadiene, acrylonitrile, methacrylic acid and graphene, is the transformed lines show of nitrile rubber latex.Good fluidity, modest viscosity, with excellent mechanical stability and chemical stability, toughness, adhesion strength are greatly improved, its product have excellent oil resistant, chemically-resistant, it is wear-resisting the features such as.
Description
Technical field
The present invention relates to rubber latex chemical technology field, specifically a kind of modified graphene nitrile rubber latex and
Its production technology.
Background technology
General, conventionally produced graphene nitrile rubber latex, its particle size not in same magnitude range, its
Mobility is not good, and viscosity is unstable, and its mechanical stability and chemical stability can not reach desired degree, its toughness, viscous
Knotting strength can not ensure well.
The content of the invention
The technical assignment of the present invention be solve the deficiencies in the prior art there is provided a kind of modified graphene nitrile rubber latex and
Its production technology.
The technical scheme is that realize in the following manner, the modified graphene nitrile rubber latex is with butadiene
With acrylonitrile be principal monomer, add graphene, using unsaturated carboxylic acid, and be aided with many double bond type cross-linking monomers and/or other
Function monomer, carries out polymerisation and obtains product, during polymerization using composite emulsifying system, i.e. reactive emulsifier and it is a small amount of cloudy from
Sub- emulsifying agent, persulfate is initiator, and alkyl hydrosulfide is molecular weight regulator, and other auxiliary agents, improves conversion ratio.
The liquid of butadiene, acrylonitrile or other reflection starting materials uses ultrasonic homogenizer used in polymerisation
Or high pressure homogenizer is scattered, the miniemulsion of 50~500nm stabilization is formed, is then added drop-wise in reactor and reacts.
The production technology of modified graphene nitrile rubber latex, the emulsion that the technique does seed using nitrile rubber latex is gathered
Technique is closed, technological process is divided into tank field flow, burden process, polymerization process, the part of cooling process four；
（1）Tank field flow
A, butadiene are delivered to butadiene storage tank；
B, acrylonitrile are transported to the storage of acrylonitrile storage tank；
（2）Burden process
A, butadiene are pumped into after butadiene caustic treater, alkali cleaning through butadiene from storage tank and are pressed onto butadiene water washing tank, after washing
It is pressed onto butadiene measuring tank standby；
B, acrylonitrile are pumped into acrylonitrile head tank from acrylonitrile storage tank through acrylonitrile, then flow automatically to acrylonitrile measuring tank standby
With；
After c, neopelex are mixed with soft water in neopelex material-compound tank, detergent alkylate is flowed automatically to
Sodium sulfonate measuring tank is standby；
D, tert-dodecylmercaotan are transported to mercaptan tank through mercaptan submerged pump, then flow automatically to mercaptan measuring tank standby；
E, potassium peroxydisulfate, graphene, additive, potassium hydroxide are standby respectively after respective material-compound tank is quantitatively mixed with soft water；
（3）Polymerization process
A, charging：Polymeric kettle leads to after nitrogen displacement, is evacuated to -0.08Mpa, starts charging, sequentially adds quantitative emulsifying agent
Sodium dodecyl benzene sulfonate aqueous solution, methacrylic acid, acrylonitrile, graphene, mercaptan, initiator, pure water, lead to nitrogen displacement two
Butadiene that is secondary, then disposably adding after quantitative processing；
B, polymerization：Stirring is opened, polymerization kettle temperature raising is to 30 DEG C, and now polymeric kettle pressure 0.4MPa, starts reaction, maintains polymeric kettle
30~35 DEG C of temperature, reacts 10 hours, then polymerization kettle temperature raising is to 60~70 DEG C, reaction 7 hours, polymerization dry in polymeric kettle
Up to more than 45%, the MPa of pressure about 0.04 in kettle after reaction, after emptying, plus nitrogen binder is to the kettle that cools；
（4）Cooling process
- 0.06MPa is vacuumized in cooling kettle, is cooled two hours, cooling kettle cools to 30 DEG C, plus potassium hydroxide aqueous solution adjusts pH8
~9, add into auxiliary agent, after sample examination is qualified, be transferred to products pot or product pond.
Produced beneficial effect is the present invention compared with prior art：
The modified graphene nitrile rubber latex is that the reaction of the materials such as butadiene, acrylonitrile, methacrylic acid and graphene gathers
Compound, is the transformed lines show of nitrile rubber latex.The consumption of reaction monomers is respectively：25-30 parts of butadiene, acrylonitrile 15-20
Part, 3-5 parts of methacrylic acid, 0.5-1 parts, one section reaction temperature of graphene are 28-40 DEG C, and second-stage reaction temperature is 50-60 DEG C.
Due to introducing carboxyl, graphene, simultaneously containing C=C double bonds, can carry out in several ways it is cross-linking vulcanized, such as sulfur cross-linking,
Peroxide cure, carboxyl dehydration crosslinking, amine vulcanization, epoxide vulcanization, diisocyanate vulcanization, radiation vulcanization, from
And various premium properties are obtained, and better than common nitrile rubber latex.
The common nitrile rubber latex of modified graphene nitrile rubber rubber ratio expands application, is widely used in aviation
The fields such as space flight, chemical industry, automobile, oil exploitation, electric wire, printing, packaging for foodstuff and weaving, be particularly suitable for use in operation hand
Set, sheath, its product tensile strength is 1.5 times of common nitrile rubber latex product, it is ensured that security reliability.
The raw material being added dropwise in production process, it is scattered using ultrasonic homogenizer or high pressure homogenizer, form 50~500nm's
Stable miniemulsion, is then added drop-wise in reactor.The graphene nitrile rubber latex produced with this method, particle size is
110~130nm, good fluidity, modest viscosity is compared with common nitrile rubber latex, with excellent mechanical stability and change
Learn stability, toughness, adhesion strength greatly improve, its product have excellent oil resistant, chemically-resistant, it is wear-resisting the features such as.
Brief description of the drawings
Accompanying drawing 1 is the reaction master equation of the present invention；
Accompanying drawing 2 is the process flow diagram of the present invention.
Embodiment
The modified graphene nitrile rubber latex and its production technology of the present invention are said in detailed below below in conjunction with the accompanying drawings
It is bright.
As shown in drawings, modified graphene nitrile rubber latex of the invention is using butadiene and acrylonitrile to be main single
Body, adds graphene, using unsaturated carboxylic acid, and is aided with many double bond type cross-linking monomers and/or other function monomers, is polymerize
Reaction obtains product, and composite emulsifying system, i.e. reactive emulsifier and a small amount of anion emulsifier, persulfate are used during polymerization
For initiator, alkyl hydrosulfide is molecular weight regulator, and other auxiliary agents, improves conversion ratio.
The liquid of butadiene, acrylonitrile or other reflection starting materials uses ultrasonic homogenizer used in polymerisation
Or high pressure homogenizer is scattered, the miniemulsion of 50~500nm stabilization is formed, is then added drop-wise in reactor and reacts.
The technique does the emulsion polymerization technique of seed using nitrile rubber latex, and technological process is divided into tank field flow, dispensing
Process, polymerization process, the part of cooling process four；
（1）Tank field flow
After a, Butadiene tanker and unloading oil filling riser connection, gas phase in butadiene storage tank is compressed to 0.7Mpa using compressor, will
Butadiene is depressed into butadiene storage tank in tank car, or utilizes butadiene unloading pump, and butadiene in tank car is delivered into butadiene storage
Tank, completes to unload；
B, acrylonitrile are pumped into the storage of acrylonitrile storage tank from tank car through acrylonitrile；
（2）Burden process
A, butadiene are pumped into after butadiene caustic treater, alkali cleaning through butadiene from storage tank and are pressed onto butadiene water washing tank, after washing
It is pressed onto butadiene measuring tank standby；
B, acrylonitrile are pumped into acrylonitrile head tank from acrylonitrile storage tank through acrylonitrile, then flow automatically to acrylonitrile measuring tank standby
With；
After c, neopelex are mixed with soft water in neopelex material-compound tank, detergent alkylate is flowed automatically to
Sodium sulfonate measuring tank is standby；
D, tert-dodecylmercaotan are transported to mercaptan tank through mercaptan submerged pump, then flow automatically to mercaptan measuring tank standby；
E, potassium peroxydisulfate, graphene, additive, potassium hydroxide are standby respectively after respective material-compound tank is quantitatively mixed with soft water；
（3）Polymerization process
A, charging：Polymeric kettle leads to after nitrogen displacement, is evacuated to -0.08Mpa, starts charging, sequentially adds quantitative emulsifying agent
Sodium dodecyl benzene sulfonate aqueous solution, methacrylic acid, acrylonitrile, graphene, mercaptan, initiator, pure water, lead to nitrogen displacement two
Butadiene that is secondary, then disposably adding after quantitative processing；
B, polymerization：Stirring is opened, jacket of polymerization leads to hot water and makes to be warming up to 30 DEG C in polymeric kettle, now polymeric kettle pressure
0.4MPa, starts reaction, leads to chilled water and maintains 30~35 DEG C of polymeric kettle temperature, reacts 10 hours, and then polymerization kettle temperature raising is to 60
~70 DEG C, react 7 hours, polymerization dry is up to more than 45% in polymeric kettle, the MPa of pressure about 0.04 in kettle after reaction, after emptying,
Plus nitrogen binder is to the kettle that cools；
The polymerisation sets DCS control systems, sets temperature of reaction kettle, pressure scene to indicate and teletransmission alarm, and and hot water
And chilled water sets interlock connection, temperature, pressure reach that emergency decompression valve guarantee polymeric kettle safety is opened in interlocking after setting value.Together
When in case of emergency, material in kettle can be transferred in cooling kettle by bottom pipeline, prevents from gathering by artificial Open valve
Kettle superpressure is closed, this project polymeric reaction temperature, rate of pressure rise are reduced with the increase in reaction time, in automatic control failure situation
Under, temperature, pressure exceed the limit value time most soon not less than 60min, and requirement is disclosure satisfy that using urgent discharging is manually operated.
（4）Cooling process
- 0.06MPa is vacuumized in cooling kettle, is cooled two hours, cooling kettle cools to 30 DEG C, plus potassium hydroxide aqueous solution adjusts pH8
~9, add into auxiliary agent, after sample examination is qualified, be transferred to products pot or product pond, progress is weighed filling.
The weight of the consumption of the reaction monomers of burden process is：25~30 parts of butadiene, 15~20 parts of acrylonitrile,
3~5 parts of methacrylic acid, 0.5~1 part of graphene, one section of reaction temperature of polymeric kettle can be 28~40 DEG C, and second-stage reaction temperature can
For 50~60 DEG C.
Claims (5)
1. modified graphene nitrile rubber latex, it is characterised in that the modified graphene nitrile rubber latex is with butadiene and third
Alkene nitrile is principal monomer, adds graphene, using unsaturated carboxylic acid, and is aided with many double bond type cross-linking monomers and/or other functions
Monomer, carries out polymerisation and obtains product, using composite emulsifying system, i.e. reactive emulsifier and a small amount of anion breast during polymerization
Agent, persulfate is initiator, and alkyl hydrosulfide is molecular weight regulator, and other auxiliary agents, improves conversion ratio.
2. modified graphene nitrile rubber latex according to claim 1, it is characterised in that：Described polymerisation is made
The liquid of butadiene, acrylonitrile or other reflection starting materials is scattered using ultrasonic homogenizer or high pressure homogenizer, shape
Into the miniemulsion of 50~500nm stabilization, then it is added drop-wise in reactor and reacts.
3. the production technology of modified graphene nitrile rubber latex, it is characterised in that：The technique is planted using nitrile rubber latex
The emulsion polymerization technique of son, technological process is divided into tank field flow, burden process, polymerization process, the part of cooling process four；
（1）Tank field flow
A, butadiene are delivered to butadiene storage tank；
B, acrylonitrile are transported to the storage of acrylonitrile storage tank；
（2）Burden process
A, butadiene are pumped into after butadiene caustic treater, alkali cleaning through butadiene from storage tank and are pressed onto butadiene water washing tank, after washing
It is pressed onto butadiene measuring tank standby；
B, acrylonitrile are pumped into acrylonitrile head tank from acrylonitrile storage tank through acrylonitrile, then flow automatically to acrylonitrile measuring tank standby
With；
After c, neopelex are mixed with soft water in neopelex material-compound tank, detergent alkylate is flowed automatically to
Sodium sulfonate measuring tank is standby；
D, tert-dodecylmercaotan are transported to mercaptan tank through mercaptan submerged pump, then flow automatically to mercaptan measuring tank standby；
E, potassium peroxydisulfate, graphene, additive, potassium hydroxide are standby respectively after respective material-compound tank is quantitatively mixed with soft water；
（3）Polymerization process
A, charging：Polymeric kettle leads to after nitrogen displacement, is evacuated to -0.08Mpa, starts charging, sequentially adds quantitative emulsifying agent
Sodium dodecyl benzene sulfonate aqueous solution, methacrylic acid, acrylonitrile, graphene, mercaptan, initiator, pure water, lead to nitrogen displacement two
Butadiene that is secondary, then disposably adding after quantitative processing；
B, polymerization：Stirring is opened, polymerization kettle temperature raising is to 30 DEG C, and now polymeric kettle pressure 0.4MPa, starts reaction, maintains polymeric kettle
30~35 DEG C of temperature, reacts 10 hours, then polymerization kettle temperature raising is to 60~70 DEG C, reaction 7 hours, polymerization dry in polymeric kettle
Up to more than 45%, the MPa of pressure about 0.04 in kettle after reaction, after emptying, plus nitrogen binder is to the kettle that cools；
（4）Cooling process
- 0.06MPa is vacuumized in cooling kettle, is cooled two hours, cooling kettle cools to 30 DEG C, plus potassium hydroxide aqueous solution adjusts pH8
~9, add into auxiliary agent, after sample examination is qualified, be transferred to products pot or product pond.
4. the production technology of modified graphene nitrile rubber latex, it is characterised in that：The technique is planted using nitrile rubber latex
The emulsion polymerization technique of son, technological process is divided into tank field flow, burden process, polymerization process, the part of cooling process four；
（1）Tank field flow
After a, Butadiene tanker and unloading oil filling riser connection, gas phase in butadiene storage tank is compressed to 0.7Mpa using compressor, will
Butadiene is depressed into butadiene storage tank in tank car, or utilizes butadiene unloading pump, and butadiene in tank car is delivered into butadiene storage
Tank, completes to unload；
B, acrylonitrile are pumped into the storage of acrylonitrile storage tank from tank car through acrylonitrile；
（2）Burden process
A, butadiene are pumped into after butadiene caustic treater, alkali cleaning through butadiene from storage tank and are pressed onto butadiene water washing tank, after washing
It is pressed onto butadiene measuring tank standby；
B, acrylonitrile are pumped into acrylonitrile head tank from acrylonitrile storage tank through acrylonitrile, then flow automatically to acrylonitrile measuring tank standby
With；
After c, neopelex are mixed with soft water in neopelex material-compound tank, detergent alkylate is flowed automatically to
Sodium sulfonate measuring tank is standby；
D, tert-dodecylmercaotan are transported to mercaptan tank through mercaptan submerged pump, then flow automatically to mercaptan measuring tank standby；
E, potassium peroxydisulfate, graphene, additive, potassium hydroxide are standby respectively after respective material-compound tank is quantitatively mixed with soft water；
（3）Polymerization process
A, charging：Polymeric kettle leads to after nitrogen displacement, is evacuated to -0.08Mpa, starts charging, sequentially adds quantitative emulsifying agent
Sodium dodecyl benzene sulfonate aqueous solution, methacrylic acid, acrylonitrile, graphene, mercaptan, initiator, pure water, lead to nitrogen displacement two
Butadiene that is secondary, then disposably adding after quantitative processing；
B, polymerization：Stirring is opened, jacket of polymerization leads to hot water and makes to be warming up to 30 DEG C in polymeric kettle, now polymeric kettle pressure
0.4MPa, starts reaction, leads to chilled water and maintains 30~35 DEG C of polymeric kettle temperature, reacts 10 hours, and then polymerization kettle temperature raising is to 60
~70 DEG C, react 7 hours, polymerization dry is up to more than 45% in polymeric kettle, the MPa of pressure about 0.04 in kettle after reaction, after emptying,
Plus nitrogen binder is to the kettle that cools；
（4）Cooling process
- 0.06MPa is vacuumized in cooling kettle, is cooled two hours, cooling kettle cools to 30 DEG C, plus potassium hydroxide aqueous solution adjusts pH8
~9, add into auxiliary agent, after sample examination is qualified, be transferred to products pot or product pond, progress is weighed filling.
5. the production technology of the modified graphene nitrile rubber latex according to claim 3 or 4, it is characterised in that：Dispensing
The weight of the consumption of the reaction monomers of process is：25~30 parts of butadiene, 15~20 parts of acrylonitrile, methacrylic acid 3
~5 parts, 0.5~1 part of graphene, one section of reaction temperature of polymeric kettle be 28~40 DEG C, second-stage reaction temperature be 50~60 DEG C.
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Cited By (6)
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|---|---|---|---|---|
| CN108598482A (en) * | 2018-04-02 | 2018-09-28 | 合肥国轩高科动力能源有限公司 | Carbon black modified water-based SBR lithium ion battery binder and preparation method thereof |
| CN109503872A (en) * | 2018-09-29 | 2019-03-22 | 武汉纺织大学 | A kind of nitrile rubber is from aggressiveness macromolecular elastomer conductive rubber and preparation method thereof |
| CN109901532A (en) * | 2019-01-25 | 2019-06-18 | 内蒙古乌海化工有限公司 | DCS system operation optimization method applied to suspension type polyvinyl-chloride production |
| CN109999723A (en) * | 2019-04-18 | 2019-07-12 | 中国科学院山西煤炭化学研究所 | Acrylonitrile raw material feed system |
| CN110183731A (en) * | 2019-06-07 | 2019-08-30 | 青岛泰歌新材料科技有限公司 | A kind of preparation method of polyaniline-modified nano-carbon material |
| CN111040190A (en) * | 2019-12-18 | 2020-04-21 | 东营九洲奥华化工有限责任公司 | Modified graphene nitrile rubber latex and production process thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108598482A (en) * | 2018-04-02 | 2018-09-28 | 合肥国轩高科动力能源有限公司 | Carbon black modified water-based SBR lithium ion battery binder and preparation method thereof |
| CN109503872A (en) * | 2018-09-29 | 2019-03-22 | 武汉纺织大学 | A kind of nitrile rubber is from aggressiveness macromolecular elastomer conductive rubber and preparation method thereof |
| CN109901532A (en) * | 2019-01-25 | 2019-06-18 | 内蒙古乌海化工有限公司 | DCS system operation optimization method applied to suspension type polyvinyl-chloride production |
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| CN110183731A (en) * | 2019-06-07 | 2019-08-30 | 青岛泰歌新材料科技有限公司 | A kind of preparation method of polyaniline-modified nano-carbon material |
| CN111040190A (en) * | 2019-12-18 | 2020-04-21 | 东营九洲奥华化工有限责任公司 | Modified graphene nitrile rubber latex and production process thereof |
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