CN110066481A - Nitrile rubber and preparation method thereof - Google Patents
Nitrile rubber and preparation method thereof Download PDFInfo
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- CN110066481A CN110066481A CN201910382589.9A CN201910382589A CN110066481A CN 110066481 A CN110066481 A CN 110066481A CN 201910382589 A CN201910382589 A CN 201910382589A CN 110066481 A CN110066481 A CN 110066481A
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- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/101—Agents modifying the decomposition temperature
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- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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Abstract
The present invention relates to field of rubber technology to provide a kind of nitrile rubber, the component including following mass fraction for the problem of the resistance to low temperature difference of nitrile rubber: 10-20 parts of nitrile rubber；12-20 parts of chlorinated paraffin；10-20 parts of naphthenic oil；6-12 parts of carbon black N550；30-40 parts of polyvinyl chloride；10-20 parts of calcium carbonate；3-10 parts of foaming agent；0.5-0.8 parts of crosslink agent DCP；Cross-linking aid 0.5-1 parts of foaming；0.2-0.5 parts of stearic acid.A kind of preparation method of nitrile rubber, comprising the following steps: S1, divide glue；S2, mixed glue；S3, a mill；S4, mixing；S5, secondary mill；S6, foaming.Cooperated by the way that polyvinyl chloride and nitrile rubber is added with certain usage ratio, by the way that raw material is added portionwise during the preparation process, be conducive to nitrile rubber it is abundant foaming and it is full cross-linked, be conducive to enhance the resilience of nitrile rubber, so that the resilience of nitrile rubber is not readily susceptible to low temperature effect, the resistance to low temperature for being conducive to improve nitrile rubber, so that the scope of application of nitrile rubber expands.
Description
Technical field
The present invention relates to field of rubber technology, more specifically, it relates to a kind of nitrile rubber and preparation method thereof.
Background technique
Nitrile rubber is as butadiene and acrylonitrile through made from emulsion polymerization, nitrile rubber mainly uses low temperature lotion
Polymerization production, oil resistivity is fabulous, wearability is high, heat resistance is preferable, bonding force is strong, has been widely used for making various oil resistants
Rubber product, a variety of oil seat gaskets, gasket, casing, flexible package, flexible rubber hose, printer's roll, cable glue material etc. are automobile, boat
Essential elastic material in the industries such as sky, petroleum, duplicating.
But the lower temperature resistance of nitrile rubber is poor, nitrile rubber is easy to become fragile at low temperature, or even is easy to follow the string,
So that nitrile rubber is dfficult to apply in low temperature field, so that the use of nitrile rubber is restricted, therefore, still there is improved sky
Between.
Summary of the invention
In view of the deficienciess of the prior art, the first object of the present invention is to provide a kind of nitrile rubber, have low
It is not easy the advantages of becoming fragile under temperature.
To achieve the above object, the present invention provides the following technical scheme that
A kind of nitrile rubber, the component including following mass fraction:
10-20 parts of nitrile rubber；
12-20 parts of chlorinated paraffin；
10-20 parts of naphthenic oil；
6-12 parts of carbon black N550；
30-40 parts of polyvinyl chloride；
10-20 parts of calcium carbonate；
3-10 parts of foaming agent；
0.5-0.8 parts of crosslink agent DCP；
Cross-linking aid 0.5-1 parts of foaming；
0.2-0.5 parts of stearic acid.
By adopting the above technical scheme, cooperated by the way that polyvinyl chloride and nitrile rubber is added with certain usage ratio, favorably
In the resistance to low temperature for improving nitrile rubber, so that nitrile rubber is not easy to become fragile in the environment of low temperature, be conducive to expand fourth
The scope of application of nitrile rubber；Pass through the amount ratio of control nitrile rubber and foaming agent, crosslink agent DCP and the cross-linking aid that foams
Example, is conducive to the full cross-linked and abundant foaming of nitrile rubber, so that the foam cell uniformity of nitrile rubber improves, thus favorably
In the resilience of raising nitrile rubber, while the resilience of nitrile rubber being made to be not readily susceptible to the influence of low temperature, is conducive to mention
The resistance to low temperature of high nitrile rubber, so that the scope of application of nitrile rubber expands.
The present invention is further arranged to: the foaming agent is azodicarbonamide.
By adopting the above technical scheme, by using azodicarbonamide as foaming agent, due to point of azodicarbonamide
It is higher to solve temperature, so that azodicarbonamide is not easy to decompose in advance in the preparation process of nitrile rubber, to be conducive to fourth
The abundant foaming of nitrile rubber is conducive to the resilience for improving nitrile rubber, makes simultaneously so that the abscess of nitrile rubber is more uniform
The resilience for obtaining nitrile rubber is not readily susceptible to the influence of low temperature, is conducive to the resistance to low temperature for improving nitrile rubber, so that fourth
The scope of application of nitrile rubber expands.
The present invention is further arranged to: the foaming cross-linking aid is zinc oxide.
By adopting the above technical scheme, by using zinc oxide as foaming cross-linking aid, zinc oxide advantageously reduces foaming
The decomposition temperature of agent so that the foaming of foaming agent is easier to be initiated, thus be conducive to foaming process to nitrile rubber and
Crosslinking mechanisms are controlled, and are conducive to the full cross-linked and abundant foaming of nitrile rubber, so that the abscess of nitrile rubber is more
Uniformly, so that the resilience for being conducive to improve nitrile rubber has so that the resilience of nitrile rubber is not readily susceptible to low temperature effect
Conducive to the resistance to low temperature for improving nitrile rubber, so that the scope of application of nitrile rubber expands.
In view of the deficienciess of the prior art, the second object of the present invention is to provide a kind of preparation side of nitrile rubber
Method has the advantages that preparing resulting nitrile rubber is not easy to become fragile at low temperature.
To achieve the above object, the present invention provides the following technical scheme that
A kind of preparation method of nitrile rubber, comprising the following steps:
S1, divide glue: nitrile rubber being squeezed in blocks；
S2, mixed glue: first polyvinyl chloride, carbon black, calcium carbonate, crosslink agent DCP, foaming cross-linking aid and stearic acid are mixed
It stirs evenly, adds chlorinated paraffin and naphthenic oil, after being uniformly mixed, S1 is added and squeezes sheet of nitrile rubber, mixes
Conjunction is formed uniformly epoxy glue and discharges；
S3, a mill: it by epoxy glue stirring, compacting, then squeezes out in flakes, forms blank；
The blank that S4, mixing: mixing S3 are formed, gradually rises smelting temperature, when temperature is up to 95 DEG C -105 DEG C, adds
Enter foaming agent, is uniformly mixed to form mixture and discharge；
S5, secondary mill: the mixture of S4 being squeezed and forms sheet stock in flakes, and control sheet stock with a thickness of 25-35mm；
S6, foaming: sheet stock being added in mold and is foamed, and control blowing temperature is 150 DEG C -165 DEG C, when control is foamed
Between be 45min-60min, be opened, it is cooling, take out foaming body to get nitrile rubber.
By adopting the above technical scheme, by first by polyvinyl chloride, carbon black, calcium carbonate, crosslink agent DCP, foaming cross-linking aid
And stearic acid is uniformly mixed, and adds chlorinated paraffin and naphthenic oil stirs evenly, each component for being conducive to nitrile rubber is mixed
Close it is more uniform, thus each component for being conducive to nitrile rubber preferably play its effect and preferably cooperate, meanwhile, pass through
Foaming agent is added when temperature is up to 95 DEG C -105 DEG C, so that foaming agent is not easy to decompose in advance, is conducive to control nitrile rubber
Foaming process carried out after crosslinking mechanisms so that the abscess of nitrile rubber is more uniform, be conducive to enhance nitrile rubber
Resilience is conducive to the resistance to low temperature for improving nitrile rubber so that the resilience of nitrile rubber is not readily susceptible to low temperature effect,
So that the scope of application of nitrile rubber expands.
The present invention is further arranged to: it is 60 DEG C -70 DEG C that sheet of temperature control is squeezed in the step S1.
By adopting the above technical scheme, it is 60 DEG C -70 DEG C by squeezing sheet of temperature in rate-determining steps S1, is conducive to butyronitrile
The each component of rubber is in half molten state, so that each component for being conducive to nitrile rubber is sufficiently mixed uniformly, so that nitrile rubber
Crosslinking it is more abundant so that the abscess of nitrile rubber is more uniform, is conducive to the resilience for improving butyronitrile, makes simultaneously
The resilience of nitrile rubber is not readily susceptible to the influence of low temperature, is conducive to the resistance to low temperature for improving nitrile rubber, so that butyronitrile
The scope of application of rubber is wider.
The present invention is further arranged to: in the step S1, logical processing thin to nitrile rubber progress 2-4 times, then discharge.
By adopting the above technical scheme, logical processing 2-4 times thin by first being carried out to nitrile rubber, then discharge, be conducive to improve
The compactness of nitrile rubber, so that being not easy that there are abscesses in nitrile rubber before foaming, to be conducive to improve nitrile rubber
Foam cell uniformity so that the resilience of nitrile rubber improves, while the resilience of nitrile rubber being made to be not readily susceptible to low temperature
Influence, be conducive to improve nitrile rubber resistance to low temperature so that the scope of application of nitrile rubber is wider.
The present invention is further arranged to: in the step S1, the thickness control for squeezing sheet of nitrile rubber is 2mm-
5mm。
By adopting the above technical scheme, by squeezed in rate-determining steps S1 sheet of nitrile rubber with a thickness of 2mm-5mm, make
Be not easy that there are abscesses in nitrile rubber before foaming, to be conducive to enhance the foam cell uniformity of nitrile rubber, so that fourth
The resilience of nitrile rubber enhances, while the resilience of nitrile rubber being made to be not readily susceptible to the influence of low temperature, is conducive to improve fourth
The resistance to low temperature of nitrile rubber, so that the scope of application of nitrile rubber is more extensive.
The present invention is further arranged to: in the step S2, being added after squeezing sheet of nitrile rubber, is gradually risen temperature
Degree, after temperature reaches 110-120 DEG C, temperature is every to increase 3 DEG C -5 DEG C, and stirring overturning epoxy glue is primary, when temperature reaches 145-155 DEG C
When, carry out epoxy glue draw operation.
By adopting the above technical scheme, sheet of temperature is squeezed by control, is conducive to the shape for controlling nitrile rubber each component
State, so that each component mixing for being conducive to nitrile rubber is more uniform, meanwhile, 3 DEG C -5 DEG C are increased by the way that temperature is every, stirring overturning
Epoxy glue is primary, is conducive to each component in epoxy glue and is sufficiently mixed uniformly, to be conducive to the full cross-linked of nitrile rubber, makes
The foam cell uniformity for obtaining nitrile rubber improves, and is conducive to the resilience for improving nitrile rubber, while making the rebound of nitrile rubber
Property is not readily susceptible to the influence of low temperature, so that the scope of application of nitrile rubber is more extensive.
The present invention is further arranged to: in the step S3, control squeeze out sheet of blank with a thickness of 1mm-3mm.
By adopting the above technical scheme, by the sheet of blank of extrusion in rate-determining steps S3 with a thickness of 1mm-3mm, so that
Be not easy that there are abscesses in blank before foaming, to be conducive to improve the compactness of blank, be conducive to improve prepare it is resulting
The foam cell uniformity of nitrile rubber so that the resilience of nitrile rubber improves, while is not easy the resilience of nitrile rubber
It is influenced by low temperature, is conducive to the resistance to low temperature for improving nitrile rubber, so that the scope of application of nitrile rubber is wider.
The present invention is further arranged to: in the step S4, after foaming agent is added, temperature is every to increase 3 DEG C -5 DEG C, and stirring is turned over
Turn mixed once material, when temperature is up to 120 DEG C -140 DEG C, carries out draw operation.
By adopting the above technical scheme, after by the way that foaming agent is added, temperature is every to increase 3 DEG C -5 DEG C, stirring overturning mixed once
Material, is conducive to foaming agent and is more uniformly scattered in mixture, to be conducive to the abundant foaming of nitrile rubber, so that butyronitrile
The abscess of rubber is more uniform, and then is conducive to improve the resilience of nitrile rubber, while making the resilience of nitrile rubber not
It is easy to be influenced by low temperature, is conducive to the resistance to low temperature for improving nitrile rubber, so that the scope of application of nitrile rubber is wider.
In conclusion the invention has the following advantages:
1. cooperating by the way that polyvinyl chloride and nitrile rubber is added with certain usage ratio, be conducive to improve nitrile rubber
Resistance to low temperature is conducive to the scope of application for expanding nitrile rubber so that nitrile rubber is not easy to become fragile in the environment of low temperature；
2. being conducive to by the usage ratio of control nitrile rubber and foaming agent, crosslink agent DCP and the cross-linking aid that foams
The resilience of nitrile rubber is improved, while the resilience of nitrile rubber being made to be not readily susceptible to the influence of low temperature, is conducive to improve
The resistance to low temperature of nitrile rubber, so that the scope of application of nitrile rubber expands；
3. equal by first mixing polyvinyl chloride, carbon black, calcium carbonate, crosslink agent DCP, foaming cross-linking aid and stearic acid
It is even, it adds chlorinated paraffin and naphthenic oil stirs evenly, each component mixing for being conducive to nitrile rubber is more uniform, meanwhile,
By adding foaming agent when temperature is up to 95 DEG C -105 DEG C, so that foaming agent is not easy to decompose in advance, be conducive to nitrile rubber
It is abundant foaming and it is full cross-linked, be conducive to enhance nitrile rubber resilience so that the resilience of nitrile rubber is not easy
By low temperature effect, be conducive to the resistance to low temperature for improving nitrile rubber, so that the scope of application of nitrile rubber expands.
Specific embodiment
With reference to embodiments, invention is further described in detail.
In following embodiment, nitrile rubber connects the nitrile rubber of the model N41 of Industrial Co., Ltd. using Shanghai three.
In following embodiment, naphthenic oil uses the cycloalkanes of the model KN4010 of Suzhou Sai Pahan specialty oil Co., Ltd
Oil 10#。
In following embodiment, carbon black N550 uses the carbon black N550 of hundred million Bo Rui Chemical Co., Ltd. of Tianjin.
In following embodiment, polyvinyl chloride uses the trade mark of the Zhou Su industry Co., Ltd of Wenzhou pleasure for the polychlorostyrene second of S-101
Alkene.
Embodiment 1
A kind of nitrile rubber, the component including following mass fraction:
Nitrile rubber 10kg；Chlorinated paraffin 14kg；Naphthenic oil 18kg；Carbon black N550 10kg；Polyvinyl chloride 38kg；Carbonic acid
Calcium 10kg；Foaming agent 10kg；Crosslink agent DCP 0.6kg；Foam cross-linking aid 0.8kg；Stearic acid 0.3kg.
In the present embodiment, foaming agent is the H foaming agent purchased from the industrial Science and Technology Ltd. of Shenzhen's marine origin.
In the present embodiment, crosslinking agent aid is silica.
Nitrile rubber the preparation method is as follows:
S1, divide glue, specific as follows:
10kg nitrile rubber is poured into two rollers of open mill, the temperature of two rollers of control is 55 DEG C, and controls the roller of two rollers
Away from for 1mm, so that the thickness for squeezing sheet of nitrile rubber is about 1mm, for use.
S2, mixed glue, specific as follows:
Carbon black N550 10kg, polyvinyl chloride 38kg, calcium carbonate 10kg, crosslink agent DCP 0.6kg, hair are added in mixer
Cross-linking aid 0.8kg, stearic acid 0.3kg are steeped, is uniformly mixed, is added chlorinated paraffin 14kg, naphthenic oil 18kg, continue to stir
It mixes uniformly mixed, adds in S1 and squeeze sheet of nitrile rubber 10kg, be uniformly mixed, form epoxy glue and simultaneously discharge.
S3, a mill, specific as follows:
Epoxy glue is poured into two rollers of open mill, the roll spacing of two rollers of control is 0.5mm, so that epoxy glue is extruded in flakes
The thickness of blank be about 0.5mm.
S4, mixing, specific as follows:
S3 is squeezed sheet of blank to be added in mixer, is stirred, and gradually rise smelting temperature, when temperature is up to 95
DEG C when, foaming agent 10kg is added, and continues to be uniformly mixed to form mixture, then carry out draw operation.
S5, secondary mill, specific as follows:
The mixture that S4 is uniformly mixed pours into two rollers of open mill, and the roll spacing of two rollers of control is 20mm, so that
The thickness for being extruded sheet of mixture is about 20mm.Sheet of mixture will be squeezed and be cut into the sheet stock that length is about 1m, and
The weight of sheet stock is weighed according to actual needs.
S6, foaming, specific as follows:
The sheet stock weighed in S5 is added in the mold of oil pressure foaming machine and is foamed, the temperature for controlling moulded from foam is
145 DEG C, the time for controlling moulded from foam is 65min, and after the completion of foaming, foaming body is taken out in die sinking, cooling to get nitrile rubber.
Embodiment 2
A kind of nitrile rubber, the component including following mass fraction:
Nitrile rubber 15kg；Chlorinated paraffin 20kg；Naphthenic oil 13kg；Carbon black N550 8kg；Polyvinyl chloride 33kg；Calcium carbonate
15kg；Foaming agent 6kg；Crosslink agent DCP 0.7kg；Foam cross-linking aid 0.5kg；Stearic acid 0.2kg.
In the present embodiment, foaming agent is the H foaming agent purchased from the industrial Science and Technology Ltd. of Shenzhen's marine origin.
In the present embodiment, crosslinking agent aid is silica.
Nitrile rubber the preparation method is as follows:
S1, divide glue, specific as follows:
15kg nitrile rubber is poured into two rollers of open mill, the temperature of two rollers of control is 75 DEG C, and controls the roller of two rollers
Away from for 6mm, so that the thickness for squeezing sheet of nitrile rubber is about 6mm, for use.
S2, mixed glue, specific as follows:
Carbon black N550 8kg, polyvinyl chloride 33kg, calcium carbonate 15kg, crosslink agent DCP 0.7kg, hair are added in mixer
Cross-linking aid 0.5kg, stearic acid 0.2kg are steeped, is uniformly mixed, is added chlorinated paraffin 20kg, naphthenic oil 13kg, continue to stir
It mixes uniformly mixed, adds in S1 and squeeze sheet of nitrile rubber 15kg, be uniformly mixed, form epoxy glue and simultaneously discharge.
S3, a mill, specific as follows:
Epoxy glue is poured into two rollers of open mill, control two rollers roll spacing be 4mm so that epoxy glue be extruded it is sheet of
The thickness of blank is about 4mm.
S4, mixing, specific as follows:
S3 is squeezed sheet of blank to be added in mixer, is stirred, and gradually rise smelting temperature, when temperature reaches
At 105 DEG C, foaming agent 6kg is added, and continue to be uniformly mixed to form mixture, then carry out draw operation.
S5, secondary mill, specific as follows:
The mixture that S4 is uniformly mixed pours into two rollers of open mill, and the roll spacing of two rollers of control is 40mm, so that
The thickness for being extruded sheet of mixture is about 40mm.Sheet of mixture will be squeezed and be cut into the sheet stock that length is about 1m, and
The weight of sheet stock is weighed according to actual needs.
S6, foaming, specific as follows:
The sheet stock weighed in S5 is added in the mold of oil pressure foaming machine and is foamed, the temperature for controlling moulded from foam is
170 DEG C, the time for controlling moulded from foam is 40min, and after the completion of foaming, foaming body is taken out in die sinking, cooling to get nitrile rubber.
Embodiment 3
A kind of nitrile rubber, the component including following mass fraction:
Nitrile rubber 20kg；Chlorinated paraffin 12kg；Naphthenic oil 10kg；Carbon black N550 12kg；Polyvinyl chloride 30kg；Carbonic acid
Calcium 20kg；Foaming agent 7kg；Crosslink agent DCP 0.6kg；Foam cross-linking aid 0.7kg；Stearic acid 0.4kg.
In the present embodiment, foaming agent is the azo dimethyl that the article No. purchased from Jiangsu Suo Pu Chemical Co., Ltd. is DN10
Amide.
In the present embodiment, foaming cross-linking aid is zinc oxide.
Nitrile rubber the preparation method is as follows:
S1, divide glue, specific as follows:
20kg nitrile rubber is poured into two rollers of open mill, the temperature of two rollers of control is 60 DEG C, and controls the roller of two rollers
Away from for 2mm so that the thickness for squeezing sheet of nitrile rubber is about 2mm, and will squeeze sheet of nitrile rubber be reentered into
In two rollers of open mill, the thin logical processing of progress 2 times, then discharge stand-by.
S2, mixed glue, specific as follows:
Carbon black N550 12kg, polyvinyl chloride 30kg, calcium carbonate 20kg, crosslink agent DCP 0.6kg, hair are added in mixer
Steep cross-linking aid 0.7kg, stearic acid 0.4kg, push pressurization lid so that feeding inlet close, while make pressurization lid not with raw material
Contact, so that after mixer idle running 25s, then it is stirred operation.
After raw material is uniformly mixed, stop stirring, and lift pressurization lid, chlorinated paraffin 12kg, naphthenic oil 10kg be added,
Pressurization lid is pushed, so that feeding inlet is closed, while pressurization lid is not contacted with raw material, the 30s so that mixer dallies, then lift
Pressurization lid is added in S1 and squeezes sheet of nitrile rubber 20kg to form epoxy glue, pushes pressurization lid so that pressurization lid with mix
Glue abuts, and is stirred to epoxy glue, while gradually rising temperature.When temperature is up to 110 DEG C, partially lifts pressurization lid, make
It is not contacted with epoxy glue while obtaining pressurization lid closing feed inlet, after pressurization lid surrounding is cleaned up, pushes pressurization lid and make
Pressurization lid abuts with epoxy glue and continues to stir.Hereafter, temperature is every rises 3 DEG C, first lifts pressurization cover and by its periphery
It cleans up, then lifts pressurization lid completely, so that feed inlet is opened, stirring overturning epoxy glue is primary.When temperature is up to 145 DEG C,
Carry out the draw operation of epoxy glue.
S3, a mill, specific as follows:
Epoxy glue is poured into two rollers of the open mill that roller diameter is 18 cun, the roll spacing of two rollers of control is 1.5mm, so that mixed
Closing glue and being extruded in flakes is about 1.5mm with the thickness of the blank of formation；It will be again to discharge in 18 cun of open mill from roller diameter
Blank is drawn in two rollers of the open mill for being 16 cun to roller diameter, and the roll spacing for the open mill that control roller diameter is 16 cun is 1mm, is made
The thickness for obtaining the blank finally to discharge is about 1mm.
S4, mixing, specific as follows:
S3 is squeezed sheet of blank to be added in mixer, pressurization lid is pushed, so that pressurization lid is contacted with blank, and stirs
Blank is mixed, while gradually rising smelting temperature, when temperature is up to 95 DEG C, first partially lifts pressurization lid, so that pressurization lid and base
Material separation, after pressurization lid periphery is cleaned up, then lifts pressurization lid completely, so that feed inlet is opened, foaming agent 6kg is added,
Pressurization lid is then pushed, so that pressurization lid is abutted with blank, continues to stir blank.Hereafter, temperature is every increases 3 DEG C, first will pressurization
Cover lifts and cleans up its periphery, then lifts pressurization lid completely, so that feed inlet is opened, stirring overturning blank one
It is secondary.After mixing evenly, mixture is formed.When temperature is up to 120 DEG C, the draw operation of mixture is carried out.
S5, secondary mill, specific as follows:
The mixture that S4 is uniformly mixed pours into two rollers of the open mill that roller diameter is 18 cun, controls the roller of two rollers
Away from for 1.5mm, so that the thickness for being extruded sheet of mixture is about 1.5mm；It again will be from the open mill that roller diameter is 18 cun
The sheet mixture of discharging is drawn in two rollers of the open mill for being 16 cun to roller diameter, the open mill that control roller diameter is 16 cun
Roll spacing is 25mm, so that the thickness of the sheet mixture finally to discharge is about 25mm.The sheet that will be discharged from 16 cun of open mills
Mixture is cut into the sheet stock that length is about 1m, and weighs the weight of sheet stock according to actual needs.
S6, foaming, specific as follows:
The sheet stock weighed in S5 is added in the mold of oil pressure foaming machine and is foamed, the temperature for controlling moulded from foam is
150 DEG C, the time for controlling moulded from foam is 60min, and after the completion of foaming, foaming body is taken out in die sinking, cooling to get nitrile rubber.
Embodiment 4
A kind of nitrile rubber, the component including following mass fraction:
Nitrile rubber 13kg；Chlorinated paraffin 16kg；Naphthenic oil 15kg；Carbon black N550 9kg；Polyvinyl chloride 40kg；Calcium carbonate
18kg；Foaming agent 8kg；Crosslink agent DCP 0.8kg；Foam cross-linking aid 0.9kg；Stearic acid 0.5kg.
In the present embodiment, foaming agent is the azo dimethyl that the article No. purchased from Jiangsu Suo Pu Chemical Co., Ltd. is DN10
Amide.
In the present embodiment, foaming cross-linking aid is zinc oxide.
Nitrile rubber the preparation method is as follows:
S1, divide glue, specific as follows:
13kg nitrile rubber is poured into two rollers of open mill, the temperature of two rollers of control is 65 DEG C, and controls the roller of two rollers
Away from for 3.5mm, so that the thickness for squeezing sheet of nitrile rubber is about 3.5mm, and sheet of nitrile rubber will be squeezed and relay
Enter into two rollers of open mill, the thin logical processing of progress 3 times, then discharges stand-by.
S2, mixed glue, specific as follows:
Carbon black N550 9kg, polyvinyl chloride 40kg, calcium carbonate 18kg, crosslink agent DCP 0.8kg, hair are added in mixer
Steep cross-linking aid 0.9kg, stearic acid 0.5kg, push pressurization lid so that feeding inlet close, while make pressurization lid not with raw material
Contact, so that after mixer idle running 30s, then it is stirred operation.
After raw material is uniformly mixed, stop stirring, and lift pressurization lid, chlorinated paraffin 16kg, naphthenic oil 15kg be added,
Pressurization lid is pushed, so that feeding inlet is closed, while pressurization lid is not contacted with raw material, the 35s so that mixer dallies, then lift
Pressurization lid is added in S1 and squeezes sheet of nitrile rubber 13kg to form epoxy glue, pushes pressurization lid so that pressurization lid with mix
Glue abuts, and is stirred to epoxy glue, while gradually rising temperature.When temperature is up to 115 DEG C, partially lifts pressurization lid, make
It is not contacted with epoxy glue while obtaining pressurization lid closing feed inlet, after pressurization lid surrounding is cleaned up, pushes pressurization lid and make
Pressurization lid abuts with epoxy glue and continues to stir.Hereafter, temperature is every rises 5 DEG C, first lifts pressurization cover and by its periphery
It cleans up, then lifts pressurization lid completely, so that feed inlet is opened, stirring overturning epoxy glue is primary.When temperature is up to 150 DEG C,
Carry out the draw operation of epoxy glue.
S3, a mill, specific as follows:
Epoxy glue is poured into two rollers of the open mill that roller diameter is 18 cun, the roll spacing of two rollers of control is 1mm, so that mixing
It is about 1mm with the thickness of the blank of formation that glue, which is extruded in flakes,；The blank that will be discharged from the open mill that roller diameter is 18 cun again
In two rollers for drawing the open mill for being 16 cun to roller diameter, the roll spacing for the open mill that control roller diameter is 16 cun is 2mm, so that most
The thickness of the blank to discharge eventually is about 2mm.
S4, mixing, specific as follows:
S3 is squeezed sheet of blank to be added in mixer, pressurization lid is pushed, so that pressurization lid is contacted with blank, and stirs
Blank is mixed, while gradually rising smelting temperature, when temperature is up to 100 DEG C, first partially lifts pressurization lid, so that pressurization lid and base
Material separation, after pressurization lid periphery is cleaned up, then lifts pressurization lid completely, so that feed inlet is opened, foaming agent 8kg is added,
Pressurization lid is then pushed, so that pressurization lid is abutted with blank, continues to stir blank.Hereafter, temperature is every increases 4 DEG C, first will pressurization
Cover lifts and cleans up its periphery, then lifts pressurization lid completely, so that feed inlet is opened, stirring overturning blank one
It is secondary.After mixing evenly, mixture is formed.When temperature is up to 130 DEG C, the draw operation of mixture is carried out.
S5, secondary mill, specific as follows:
The mixture that S4 is uniformly mixed pours into two rollers of the open mill that roller diameter is 18 cun, controls the roller of two rollers
Away from for 1.5mm, so that the thickness for being extruded sheet of mixture is about 1.5mm；It again will be from the open mill that roller diameter is 18 cun
The sheet mixture of discharging is drawn in two rollers of the open mill for being 16 cun to roller diameter, the open mill that control roller diameter is 16 cun
Roll spacing is 30mm, so that the thickness of the sheet mixture finally to discharge is about 30mm.The sheet that will be discharged from 16 cun of open mills
Mixture is cut into the sheet stock that length is about 1m, and weighs the weight of sheet stock according to actual needs.
S6, foaming, specific as follows:
The sheet stock weighed in S5 is added in the mold of oil pressure foaming machine and is foamed, the temperature for controlling moulded from foam is
158 DEG C, the time for controlling moulded from foam is 53min, and after the completion of foaming, foaming body is taken out in die sinking, cooling to get nitrile rubber.
Embodiment 5
A kind of nitrile rubber, the component including following mass fraction:
Nitrile rubber 18kg；Chlorinated paraffin 18kg；Naphthenic oil 20kg；Carbon black N550 6kg；Polyvinyl chloride 35kg；Calcium carbonate
13kg；Foaming agent 3kg；Crosslink agent DCP 0.5kg；Foam cross-linking aid 1kg；Stearic acid 0.3kg.
In the present embodiment, foaming agent is the azo dimethyl that the article No. purchased from Jiangsu Suo Pu Chemical Co., Ltd. is DN10
Amide.
In the present embodiment, foaming cross-linking aid is zinc oxide.
Nitrile rubber the preparation method is as follows:
S1, divide glue, specific as follows:
18kg nitrile rubber is poured into two rollers of open mill, the temperature of two rollers of control is 70 DEG C, and controls the roller of two rollers
Away from for 5mm so that the thickness for squeezing sheet of nitrile rubber is about 5mm, and will squeeze sheet of nitrile rubber be reentered into
In two rollers of open mill, the thin logical processing of progress 4 times, then discharge stand-by.
S2, mixed glue, specific as follows:
Carbon black N550 6kg, polyvinyl chloride 35kg, calcium carbonate 13kg, crosslink agent DCP 0.5kg, hair are added in mixer
Cross-linking aid 1kg, stearic acid 0.3kg are steeped, pressurization lid is pushed, so that feeding inlet is closed, while pressurization lid is not connect with raw material
Touching, so that after mixer idle running 35s, then it is stirred operation.
After raw material is uniformly mixed, stop stirring, and lift pressurization lid, chlorinated paraffin 18kg, naphthenic oil 20kg be added,
Pressurization lid is pushed, so that feeding inlet is closed, while pressurization lid is not contacted with raw material, the 25s so that mixer dallies, then lift
Pressurization lid is added in S1 and squeezes sheet of nitrile rubber 18kg to form epoxy glue, pushes pressurization lid so that pressurization lid with mix
Glue abuts, and is stirred to epoxy glue, while gradually rising temperature.When temperature is up to 120 DEG C, partially lifts pressurization lid, make
It is not contacted with epoxy glue while obtaining pressurization lid closing feed inlet, after pressurization lid surrounding is cleaned up, pushes pressurization lid and make
Pressurization lid abuts with epoxy glue and continues to stir.Hereafter, temperature is every rises 3 DEG C, first lifts pressurization cover and by its periphery
It cleans up, then lifts pressurization lid completely, so that feed inlet is opened, stirring overturning epoxy glue is primary.When temperature is up to 155 DEG C,
Carry out the draw operation of epoxy glue.
S3, a mill, specific as follows:
Epoxy glue is poured into two rollers of the open mill that roller diameter is 18 cun, the roll spacing of two rollers of control is 1.5mm, so that mixed
Closing glue and being extruded in flakes is about 1.5mm with the thickness of the blank of formation；It will be again to discharge in 18 cun of open mill from roller diameter
Blank is drawn in two rollers of the open mill for being 16 cun to roller diameter, and the roll spacing for the open mill that control roller diameter is 16 cun is 3mm, is made
The thickness for obtaining the blank finally to discharge is about 3mm.
S4, mixing, specific as follows:
S3 is squeezed sheet of blank to be added in mixer, pressurization lid is pushed, so that pressurization lid is contacted with blank, and stirs
Blank is mixed, while gradually rising smelting temperature, when temperature is up to 105 DEG C, first partially lifts pressurization lid, so that pressurization lid and base
Material separation, after pressurization lid periphery is cleaned up, then lifts pressurization lid completely, so that feed inlet is opened, foaming agent 3kg is added,
Pressurization lid is then pushed, so that pressurization lid is abutted with blank, continues to stir blank.Hereafter, temperature is every increases 3 DEG C, first will pressurization
Cover lifts and cleans up its periphery, then lifts pressurization lid completely, so that feed inlet is opened, stirring overturning blank one
It is secondary.After mixing evenly, mixture is formed.When temperature is up to 140 DEG C, the draw operation of mixture is carried out.
S5, secondary mill, specific as follows:
The mixture that S4 is uniformly mixed pours into two rollers of the open mill that roller diameter is 18 cun, controls the roller of two rollers
Away from for 1.5mm, so that the thickness for being extruded sheet of mixture is about 1.5mm；It again will be from the open mill that roller diameter is 18 cun
The sheet mixture of discharging is drawn in two rollers of the open mill for being 16 cun to roller diameter, the open mill that control roller diameter is 16 cun
Roll spacing is 35mm, so that the thickness of the sheet mixture finally to discharge is about 35mm.The sheet that will be discharged from 16 cun of open mills
Mixture is cut into the sheet stock that length is about 1m, and weighs the weight of sheet stock according to actual needs.
S6, foaming, specific as follows:
The sheet stock weighed in S5 is added in the mold of oil pressure foaming machine and is foamed, the temperature for controlling moulded from foam is
165 DEG C, the time for controlling moulded from foam is 45min, and after the completion of foaming, foaming body is taken out in die sinking, cooling to get nitrile rubber.
Comparative example 1
Use notification number for Chinese patent document " a kind of polysiloxane-modified nitrile rubber, synthesis of CN102516558B
Embodiment 1 in the preparation of method and its vulcanizate " is used as comparative example.
Experiment 1
Above embodiments, which are detected, according to GB/T1682-1994 " the measurement single specimen method of vulcanized rubber black brittleness " prepares institute
The brittleness temperature (DEG C) of the nitrile rubber obtained.
Experiment 2
It is prepared according to GB/T6034-1985 " measurement that vulcanized rubber compresses cold-resistant coefficient " detection above embodiments resulting
Compression of the nitrile rubber at -55 DEG C is resisted cold coefficient.
Experiment 3
Above implement is detected according to GB/T1683-2018 " measuring method of vulcanized rubber constant deformation compression set "
Example prepares the compression set rate (%) of resulting nitrile rubber.
The above detection data is shown in Table 1.
Table 1
| Brittleness temperature (DEG C) | Compress cold-resistant coefficient | Compression set rate (%) | |
| Embodiment 1 | -77 | 0.481 | 6 |
| Embodiment 2 | -76 | 0.472 | 6 |
| Embodiment 3 | -85 | 0.641 | 3 |
| Embodiment 4 | -84 | 0.652 | 2 |
| Embodiment 5 | -85 | 0.643 | 2 |
| Comparative example 1 | -71 | 0.361 | 13 |
It can be obtained according to the data comparison of embodiment 1-5 in table 1 and comparative example 1, embodiment 1-5 is distributed using group of the invention
Than and preparation method prepare nitrile rubber, comparative example 1 uses prior art preparation nitrile rubber, and the brittleness of embodiment 1-5
Temperature is far below comparative example 1, and the cold-resistant coefficient of the compression of embodiment 1-5 is much higher than comparative example 1, the pressure of embodiment 1-5
Compression permanent deformation rate is far below comparative example 1, i.e. embodiment 1-5 prepares the resilience of resulting nitrile rubber and low temperature resistant
Performance is superior to comparative example 1, illustrates to prepare nitrile rubber by using component proportion and preparation method of the invention, favorably
In the foam cell uniformity for improving nitrile rubber, so that the resilience of nitrile rubber enhances, while making the resilience of nitrile rubber
It is not readily susceptible to the influence of low temperature, is conducive to the resistance to low temperature for enhancing nitrile rubber, so that the scope of application of nitrile rubber is more
Extensively.
It can be obtained according to the data comparison of embodiment 1-2 in table 1 and embodiment 3-5, embodiment 1-2 uses the BK conduct of urea rouge
Foaming agent, using silica as foaming cross-linking aid, embodiment 3-5 uses azodicarbonamide as foaming agent, using oxygen
Change zinc as foaming cross-linking aid, and embodiment 1-2 has lacked the mistake that the temperature in internal mixing pass gradually rises than embodiment 3-5
Cheng Zhong, temperature is every to rise 3 DEG C -5 DEG C, the primary operation of the mixture in stirring turnover internal mixer, meanwhile, embodiment 1-2 and reality
Apply the smelting temperature of a 3-5, the time has a certain difference, and the brittleness temperature of embodiment 3-5 is lower than embodiment 1-2,
The cold-resistant coefficient of the compression of embodiment 3-5 is lower than embodiment 1-2 higher than embodiment 1-2, the compression set rate of embodiment 3-5
, i.e., the resilience of embodiment 3-5 and resistance to low temperature are superior to embodiment 1-2, illustrate by using two formyl of azo
Amine is as foaming agent, by using zinc oxide as foaming cross-linking aid, azodicarbonamide decomposition temperature with higher, no
It is easy to decompose in advance in internal mixing pass, meanwhile, by the way that zinc oxide is added, advantageously reduce the decomposition temperature of azodicarbonamide
Degree, so that the foaming for being conducive to foaming agent causes, is conducive to the hair for controlling nitrile rubber so that the decomposition temperature of foaming agent reduces
Bubble process carries out after crosslinking mechanisms, so that the crosslinking and foaming of nitrile rubber are more abundant, is conducive to nitrile rubber friendship
Connection forms reticular structure, while making the abscess for preparing resulting nitrile rubber foaming more uniform, and then be conducive to improve fourth
The resilience and heat insulating ability of nitrile rubber, while the resilience of nitrile rubber being made to be not readily susceptible to low temperature effect, be conducive to enhance
The resistance to low temperature of nitrile rubber, so that the scope of application of nitrile rubber is wider；Pass through the raised mistake of temperature in internal mixing pass
Cheng Zhong, temperature is every to increase 3 DEG C -5 DEG C, stir mixture in turnover internal mixer primary and the temperature by controlling mixing and when
Between, each component mixing dispersion for being conducive to nitrile rubber is more uniform, to be conducive to sufficiently foaming and filling for nitrile rubber
Point crosslinking so that the resilience of nitrile rubber improves, while making the resilience of nitrile rubber be not readily susceptible to the influence of low temperature,
The resistance to low temperature for being conducive to improve nitrile rubber, so that the scope of application of nitrile rubber is wider.
The embodiment of present embodiment is presently preferred embodiments of the present invention, not limits protection of the invention according to this
Range, therefore: the equivalence changes that all structures under this invention, shape, principle are done, should all be covered by protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of nitrile rubber, it is characterized in that: including the component of following mass fraction:
10-20 parts of nitrile rubber；
12-20 parts of chlorinated paraffin；
10-20 parts of naphthenic oil；
6-12 parts of carbon black N550；
30-40 parts of polyvinyl chloride；
10-20 parts of calcium carbonate；
3-10 parts of foaming agent；
0.5-0.8 parts of crosslink agent DCP；
Cross-linking aid 0.5-1 parts of foaming；
0.2-0.5 parts of stearic acid.
2. nitrile rubber according to claim 1, it is characterized in that: the foaming agent is azodicarbonamide.
3. nitrile rubber according to claim 1 to 2, it is characterized in that: the foaming cross-linking aid is zinc oxide.
4. a kind of preparation method of nitrile rubber a method according to any one of claims 1-3, it is characterized in that: the following steps are included:
S1, divide glue: nitrile rubber being squeezed in blocks；
S2, mixed glue: first polyvinyl chloride, carbon black, calcium carbonate, crosslink agent DCP, foaming cross-linking aid and stearic acid are mixed
Uniformly, chlorinated paraffin and naphthenic oil are added, after being uniformly mixed, S1 is added and squeezes sheet of nitrile rubber, mixing is equal
Even formation epoxy glue simultaneously discharges；
S3, a mill: it by epoxy glue stirring, compacting, then squeezes out in flakes, forms blank；
The blank that S4, mixing: mixing S3 are formed, gradually rises smelting temperature, and when temperature is up to 95 DEG C -105 DEG C, hair is added
Infusion is uniformly mixed to form mixture and discharge；
S5, secondary mill: the mixture of S4 being squeezed and forms sheet stock in flakes, and control sheet stock with a thickness of 25-35mm；
S6, foaming: sheet stock being added in mold and is foamed, and control blowing temperature is 150 DEG C -165 DEG C, and control foamed time is
45min-60min is opened, cooling, takes out foaming body to get nitrile rubber.
5. the preparation method of nitrile rubber according to claim 4, it is characterized in that: being squeezed sheet of in the step S1
Temperature control is 60 DEG C -70 DEG C.
6. the preparation method of nitrile rubber according to claim 4, it is characterized in that: in the step S1, to nitrile rubber
It carries out logical processing 2-4 times thin, then discharges.
7. according to the preparation method of any nitrile rubber of claim 4-6, it is characterized in that: being squeezed in the step S1
The thickness control of sheet of nitrile rubber is 2mm-5mm.
8. according to the preparation method of any nitrile rubber of claim 4-6, it is characterized in that: being added in the step S2
After squeezing sheet of nitrile rubber, temperature is gradually risen, after temperature reaches 110-120 DEG C, temperature is every to increase 3 DEG C -5 DEG C, stirring
It is primary to overturn epoxy glue, when temperature reaches 145-155 DEG C, carries out epoxy glue draw operation.
9. according to the preparation method of any nitrile rubber of claim 4-6, it is characterized in that: in the step S3, control
Squeeze out sheet of blank with a thickness of 1mm-3mm.
10. according to the preparation method of any nitrile rubber of claim 4-6, it is characterized in that: being added in the step S4
After foaming agent, temperature is every to increase 3 DEG C -5 DEG C, and stirring overturning mixed once material discharges when temperature is up to 120 DEG C -140 DEG C
Operation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1241593A (en) * | 1998-12-31 | 2000-01-19 | 宜兴市凯凯橡塑保温材料厂 | Rubber-plastic sponge heat-insulating fireproof material and its production process |
| CN108034094A (en) * | 2017-12-28 | 2018-05-15 | 华美节能科技集团有限公司 | Without elemental sulfur rubber-plastic insulating thermal insulation material and preparation method thereof |
| CN109337240A (en) * | 2018-09-18 | 2019-02-15 | 江苏理工学院 | A kind of environmental protection flame retardant PVC/NBR foamed material and preparation method thereof |
| CN109400990A (en) * | 2018-12-17 | 2019-03-01 | 班倍(上海)工业技术有限公司 | A kind of rubber-plastic heat insulation material essence control technique |
-
2019
- 2019-05-09 CN CN201910382589.9A patent/CN110066481B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1241593A (en) * | 1998-12-31 | 2000-01-19 | 宜兴市凯凯橡塑保温材料厂 | Rubber-plastic sponge heat-insulating fireproof material and its production process |
| CN108034094A (en) * | 2017-12-28 | 2018-05-15 | 华美节能科技集团有限公司 | Without elemental sulfur rubber-plastic insulating thermal insulation material and preparation method thereof |
| CN109337240A (en) * | 2018-09-18 | 2019-02-15 | 江苏理工学院 | A kind of environmental protection flame retardant PVC/NBR foamed material and preparation method thereof |
| CN109400990A (en) * | 2018-12-17 | 2019-03-01 | 班倍(上海)工业技术有限公司 | A kind of rubber-plastic heat insulation material essence control technique |
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