CN110066481B - Nitrile rubber and preparation method thereof - Google Patents
Nitrile rubber and preparation method thereof Download PDFInfo
- Publication number
- CN110066481B CN110066481B CN201910382589.9A CN201910382589A CN110066481B CN 110066481 B CN110066481 B CN 110066481B CN 201910382589 A CN201910382589 A CN 201910382589A CN 110066481 B CN110066481 B CN 110066481B
- Authority
- CN
- China
- Prior art keywords
- nitrile rubber
- foaming
- rubber
- mixing
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2409/02—Copolymers with acrylonitrile
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to the technical field of rubber, and provides a nitrile rubber aiming at the problem of poor low-temperature resistance of the nitrile rubber, which comprises the following components in parts by mass: 10-20 parts of nitrile rubber; 12-20 parts of chlorinated paraffin; 10-20 parts of naphthenic oil; carbon black N5506-12 shares; 30-40 parts of polyvinyl chloride; 10-20 parts of calcium carbonate; 3-10 parts of a foaming agent; 0.5-0.8 part of DCP serving as a crosslinking agent; 0.5-1 part of foaming crosslinking auxiliary agent; 0.2-0.5 part of stearic acid. A preparation method of nitrile rubber comprises the following steps: s1, separating glue; s2, mixing the glue; s3, primary open mixing; s4, mixing and stirring; s5, secondary open mixing; s6, foaming. Through adding polyvinyl chloride and nitrile rubber and coordinating with certain quantity proportion, through adding the raw materials in batches in the preparation process, be favorable to nitrile rubber's abundant foaming and abundant crosslinking, be favorable to strengthening nitrile rubber's resilience for nitrile rubber's resilience is difficult to receive low temperature and influences, is favorable to improving nitrile rubber's low temperature resistant performance, makes nitrile rubber's application scope expand.
Description
Technical Field
The invention relates to the technical field of rubber, in particular to nitrile rubber and a preparation method thereof.
Background
The nitrile rubber is prepared from butadiene and acrylonitrile by an emulsion polymerization method, is mainly produced by a low-temperature emulsion polymerization method, has excellent oil resistance, extremely high wear resistance, better heat resistance and strong bonding force, is widely used for manufacturing various oil-resistant rubber products, various oil-resistant gaskets, sleeves, flexible packages, flexible rubber tubes, printing and dyeing rubber rollers, cable rubber materials and the like, and is an essential elastic material in the industries of automobiles, aviation, petroleum, copying and the like.
However, nitrile rubbers have poor low temperature resistance, and nitrile rubbers are easily embrittled and even easily lose elasticity at low temperatures, so that nitrile rubbers are difficult to apply in the low temperature field, and the use of nitrile rubbers is limited, and thus, there is still room for improvement.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a nitrile rubber which has the advantage of not being easy to become brittle at low temperature.
In order to achieve the purpose, the invention provides the following technical scheme:
the nitrile rubber comprises the following components in parts by mass:
10-20 parts of nitrile rubber;
12-20 parts of chlorinated paraffin;
10-20 parts of naphthenic oil;
carbon black N5506-12 shares;
30-40 parts of polyvinyl chloride;
10-20 parts of calcium carbonate;
3-10 parts of a foaming agent;
0.5-0.8 part of DCP serving as a crosslinking agent;
0.5-1 part of foaming crosslinking auxiliary agent;
0.2-0.5 part of stearic acid.
By adopting the technical scheme, the polyvinyl chloride is added to be matched with the nitrile rubber in a certain dosage proportion, so that the low-temperature resistance of the nitrile rubber is favorably improved, the nitrile rubber is not easy to become brittle in a low-temperature environment, and the application range of the nitrile rubber is favorably expanded; by controlling the dosage proportion of the nitrile rubber, the foaming agent, the cross-linking agent DCP and the foaming cross-linking auxiliary agent, the full cross-linking and the full foaming of the nitrile rubber are facilitated, the foam uniformity of the nitrile rubber is improved, the rebound resilience of the nitrile rubber is not influenced by low temperature easily, the low-temperature resistance of the nitrile rubber is facilitated to be improved, and the application range of the nitrile rubber is enlarged.
The invention is further configured to: the foaming agent is azodicarbonamide.
Adopt above-mentioned technical scheme, through adopting azo-bis formamide as the foamer, because azo-bis formamide's decomposition temperature is higher, make azo-bis formamide be difficult to decompose in advance in butadiene acrylonitrile rubber's preparation process, thereby be favorable to butadiene acrylonitrile rubber's abundant foaming, make butadiene acrylonitrile rubber's bubble more even, be favorable to improving butadiene acrylonitrile rubber's resilience, make butadiene acrylonitrile rubber's resilience be difficult to receive microthermal influence simultaneously, be favorable to improving butadiene acrylonitrile rubber's low temperature resistance, make butadiene acrylonitrile rubber's application scope expand.
The invention is further configured to: the foaming crosslinking auxiliary agent is zinc oxide.
Adopt above-mentioned technical scheme, through adopting zinc oxide as foaming cross-linking auxiliary agent, zinc oxide is favorable to reducing the decomposition temperature of foamer, make the foaming of foamer triggered more easily, thereby be favorable to controlling nitrile rubber's foaming process and crosslinking process, be favorable to nitrile rubber's abundant crosslinking and abundant foaming, make nitrile rubber's bubble more even, thereby be favorable to improving nitrile rubber's resilience, make nitrile rubber's resilience be difficult to receive the low temperature and influence, be favorable to improving nitrile rubber's low temperature resistance ability, make nitrile rubber's application scope expand.
Aiming at the defects in the prior art, the second purpose of the invention is to provide a preparation method of nitrile rubber, which has the advantage that the prepared nitrile rubber is not easy to become brittle at low temperature.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of nitrile rubber comprises the following steps:
s1, glue separation: extruding nitrile rubber into sheets;
s2, mixing rubber: firstly, mixing and stirring polyvinyl chloride, carbon black, calcium carbonate, a crosslinking agent DCP, a foaming crosslinking aid and stearic acid uniformly, then adding chlorinated paraffin and naphthenic oil, stirring and mixing uniformly, then adding S1 to extrude into sheets of nitrile rubber, mixing uniformly to form mixed rubber, and discharging;
s3, primary open mixing: stirring and compacting the mixed glue, and extruding into sheets to form blanks;
s4, mixing and stirring: carrying out banburying on the blank formed by the S3, gradually raising the banburying temperature, adding a foaming agent when the temperature reaches 95-105 ℃, uniformly stirring and mixing to form a mixture, and discharging;
s5, secondary open mixing: extruding the mixture of S4 into sheets to form sheet materials, and controlling the thickness of the sheet materials to be 25-35 mm;
s6, foaming: and adding the sheet material into a mold for foaming, controlling the foaming temperature to be 150-165 ℃, controlling the foaming time to be 45-60 min, opening the mold, cooling, and taking out the foaming body to obtain the nitrile rubber.
By adopting the technical scheme, polyvinyl chloride, carbon black, calcium carbonate, a cross-linking agent DCP, a foaming cross-linking auxiliary agent and stearic acid are uniformly mixed, chlorinated paraffin and naphthenic oil are added and uniformly stirred, so that the components of the nitrile rubber are uniformly mixed, the components of the nitrile rubber can be better exerted and better matched, meanwhile, the foaming agent is added when the temperature reaches 95-105 ℃, the foaming agent is not easily decomposed in advance, the foaming process of the nitrile rubber can be controlled after the cross-linking process, the foam pores of the nitrile rubber are more uniform, the rebound resilience of the nitrile rubber can be enhanced, the rebound resilience of the nitrile rubber is not easily influenced by low temperature, the low-temperature resistance of the nitrile rubber can be improved, and the application range of the nitrile rubber can be expanded.
The invention is further configured to: the temperature of the extruded sheet in the step S1 is controlled to be 60-70 ℃.
By adopting the technical scheme, the temperature of the extruded sheet in the step S1 is controlled to be 60-70 ℃, each component which is beneficial to the nitrile rubber is in a semi-molten state, so that each component which is beneficial to the nitrile rubber is fully mixed uniformly, the cross-linking of the nitrile rubber is more sufficient, and the foam holes of the nitrile rubber are more uniform, the rebound resilience of the nitrile rubber is beneficial to being improved, meanwhile, the rebound resilience of the nitrile rubber is not easy to be influenced by low temperature, the low temperature resistance of the nitrile rubber is beneficial to being improved, and the application range of the nitrile rubber is wider.
The invention is further configured to: in the step S1, the nitrile rubber is subjected to thin-pass treatment for 2 to 4 times and then discharged.
Adopt above-mentioned technical scheme, through carrying out thin logical processing 2-4 times to butadiene acrylonitrile rubber earlier, the ejection of compact degree that is favorable to improving butadiene acrylonitrile rubber for be difficult to have the bubble before the inherent foaming of butadiene acrylonitrile rubber, thereby be favorable to improving butadiene acrylonitrile rubber's bubble degree of consistency, make butadiene acrylonitrile rubber's resilience improve, make butadiene acrylonitrile rubber's resilience be difficult to receive microthermal influence simultaneously, be favorable to improving butadiene acrylonitrile rubber's low temperature resistance ability, make butadiene acrylonitrile rubber's application scope wider.
The invention is further configured to: in the step S1, the thickness of the nitrile rubber extruded into the sheet is controlled to be 2mm-5 mm.
By adopting the technical scheme, the thickness of the acrylonitrile-butadiene rubber extruded into the sheets in the step S1 is controlled to be 2-5 mm, so that the pores are difficult to exist before the acrylonitrile-butadiene rubber is foamed, the uniformity of the pores of the acrylonitrile-butadiene rubber is enhanced, the resilience of the acrylonitrile-butadiene rubber is difficult to be influenced by low temperature, the low-temperature resistance of the acrylonitrile-butadiene rubber is improved, and the application range of the acrylonitrile-butadiene rubber is wider.
The invention is further configured to: in the step S2, the temperature is gradually increased after the nitrile rubber extruded into the sheet is added, when the temperature reaches 110-120 ℃, the temperature is increased by 3-5 ℃ every time the temperature is increased, the mixed rubber is stirred and overturned once, and when the temperature reaches 145-155 ℃, the mixed rubber discharging operation is carried out.
Adopt above-mentioned technical scheme, through the temperature of control extrusion piece, be favorable to controlling the state of each component of butadiene-acrylonitrile rubber, thereby be favorable to each component of butadiene-acrylonitrile rubber to mix more evenly, and simultaneously, through every 3 ℃ -5 ℃ that rises of temperature, the stirring upset miscella is once, be favorable to each component intensive mixing in the miscella, thereby be favorable to butadiene-acrylonitrile rubber's abundant cross-linking, make butadiene-acrylonitrile rubber's bubble degree of consistency improve, be favorable to improving butadiene-acrylonitrile rubber's resilience, make butadiene-acrylonitrile rubber's resilience be difficult to receive microthermal influence simultaneously, make butadiene-acrylonitrile rubber's application scope more extensive.
The invention is further configured to: in the step S3, the thickness of the extruded sheet billet is controlled to be 1mm-3 mm.
By adopting the technical scheme, the thickness of the extruded flaky blank in the step S3 is controlled to be 1-3 mm, so that the bubble is difficult to exist before the blank is foamed, the compactness of the blank is improved, the uniformity of the bubble of the nitrile rubber obtained by preparation is improved, the resilience of the nitrile rubber is difficult to be influenced by low temperature, the low-temperature resistance of the nitrile rubber is improved, and the application range of the nitrile rubber is wider.
The invention is further configured to: in the step S4, after the foaming agent is added, the mixture is stirred and overturned once when the temperature rises to 3-5 ℃, and when the temperature reaches 120-140 ℃, the discharging operation is carried out.
By adopting the technical scheme, after the foaming agent is added, the temperature rises by 3-5 ℃ every time, the mixture is stirred and overturned once, so that the foaming agent is favorably and uniformly dispersed in the mixture, the full foaming of the nitrile rubber is favorably realized, the foam holes of the nitrile rubber are more uniform, the rebound resilience of the nitrile rubber is favorably improved, the rebound resilience of the nitrile rubber is difficultly influenced by low temperature, the low temperature resistance of the nitrile rubber is favorably improved, and the application range of the nitrile rubber is wider.
In conclusion, the invention has the following beneficial effects:
1. by adding the polyvinyl chloride and the nitrile rubber in a certain dosage proportion, the low-temperature resistance of the nitrile rubber is favorably improved, so that the nitrile rubber is not easy to become brittle in a low-temperature environment, and the application range of the nitrile rubber is favorably expanded;
2. by controlling the dosage proportion of the nitrile rubber, the foaming agent, the cross-linking agent DCP and the foaming cross-linking auxiliary agent, the rebound resilience of the nitrile rubber is favorably improved, and meanwhile, the rebound resilience of the nitrile rubber is not easily influenced by low temperature, the low temperature resistance of the nitrile rubber is favorably improved, and the application range of the nitrile rubber is expanded;
3. polyvinyl chloride, carbon black, calcium carbonate, a crosslinking agent DCP, a foaming crosslinking assistant and stearic acid are uniformly mixed at first, chlorinated paraffin and naphthenic oil are added and uniformly stirred, so that the components of the nitrile rubber are uniformly mixed, meanwhile, the foaming agent is added when the temperature reaches 95-105 ℃, so that the foaming agent is not easily decomposed in advance, the full foaming and the full crosslinking of the nitrile rubber are facilitated, the rebound resilience of the nitrile rubber is favorably enhanced, the rebound resilience of the nitrile rubber is not easily influenced by low temperature, the low temperature resistance of the nitrile rubber is favorably improved, and the application range of the nitrile rubber is expanded.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, the nitrile rubber used was nitrile rubber available from Shanghai Sanlian industries, Ltd.No. N41.
In the following examples, naphthenic oil 10 of KN4010 from Special oils Ltd of Seapahan, Suzhou was used as the naphthenic oil#。
In the following examples, carbon black N550 manufactured by Tianjin Yibo chemical Co., Ltd was used as carbon black N550.
In the following examples, polyvinyl chloride of the Wenzhou Leizhou plastics Co., Ltd is used under the trade name S-101.
Example 1
The nitrile rubber comprises the following components in parts by mass:
10kg of nitrile rubber; 14kg of chlorinated paraffin; 18kg of naphthenic oil; carbon black N55010 kg; 38kg of polyvinyl chloride; 10kg of calcium carbonate; 10kg of foaming agent; 0.6kg of cross-linking agent DCP; 0.8kg of foaming crosslinking auxiliary agent; stearic acid 0.3 kg.
In this example, the foaming agent is an H foaming agent purchased from Shenzhen Shencheng science and technology Limited.
In this embodiment, the crosslinker adjunct is silica.
The preparation method of the nitrile rubber comprises the following steps:
s1, separating the glue, which is specifically as follows:
10kg of nitrile rubber is poured into two rollers of an open mill, the temperature of the two rollers is controlled to be 55 ℃, and the roller spacing of the two rollers is controlled to be 1mm, so that the thickness of the nitrile rubber extruded into a sheet is about 1mm for later use.
S2, mixing the rubber, specifically as follows:
adding carbon black N55010 kg, 38kg of polyvinyl chloride, 10kg of calcium carbonate, 0.6kg of cross-linking agent DCP, 0.8kg of foaming cross-linking aid and 0.3kg of stearic acid into an internal mixer, stirring and mixing uniformly, then adding 14kg of chlorinated paraffin and 18kg of naphthenic oil, continuing stirring and mixing uniformly, then adding 10kg of butadiene-acrylonitrile rubber extruded into sheets in S1, stirring and mixing uniformly to form mixed rubber, and discharging.
S3, primary open mixing, which comprises the following steps:
pouring the mixed glue into two rollers of an open mill, and controlling the roller spacing of the two rollers to be 0.5mm, so that the thickness of the blank extruded into the sheet by the mixed glue is about 0.5 mm.
S4, mixing and stirring, specifically comprising the following steps:
adding the blank extruded into the sheet by the S3 into an internal mixer, stirring and mixing, gradually raising the internal mixing temperature, adding 10kg of foaming agent when the temperature reaches 95 ℃, continuously stirring and uniformly mixing to form a mixture, and then carrying out discharging operation.
S5, secondary open mixing, which comprises the following steps:
and pouring the mixture which is stirred and mixed uniformly in the S4 process into two rollers of an open mill, and controlling the roller spacing of the two rollers to be 20mm, so that the thickness of the mixture which is extruded into a sheet is about 20 mm. The mixture extruded into tablets was cut into pieces having a length of about 1m, and the pieces were weighed as needed.
S6, foaming, specifically comprising the following steps:
and (3) adding the weighed sheet materials in the S5 into a die of an oil pressure foaming machine for foaming, controlling the temperature of die pressing foaming to be 145 ℃, controlling the time of die pressing foaming to be 65min, opening the die after foaming is finished, taking out the foaming body, and cooling to obtain the nitrile rubber.
Example 2
The nitrile rubber comprises the following components in parts by mass:
15kg of nitrile rubber; 20kg of chlorinated paraffin; 13kg of naphthenic oil; carbon black N5508 kg; 33kg of polyvinyl chloride; 15kg of calcium carbonate; 6kg of foaming agent; 0.7kg of cross-linking agent DCP; 0.5kg of foaming crosslinking auxiliary agent; stearic acid 0.2 kg.
In this example, the foaming agent is an H foaming agent purchased from Shenzhen Shencheng science and technology Limited.
In this embodiment, the crosslinker adjunct is silica.
The preparation method of the nitrile rubber comprises the following steps:
s1, separating the glue, which is specifically as follows:
15kg of nitrile rubber is poured into two rollers of an open mill, the temperature of the two rollers is controlled to be 75 ℃, and the roller spacing of the two rollers is controlled to be 6mm, so that the thickness of the nitrile rubber extruded into a sheet is about 6mm for later use.
S2, mixing the rubber, specifically as follows:
adding carbon black N5508 kg, 33kg of polyvinyl chloride, 15kg of calcium carbonate, 0.7kg of cross-linking agent DCP, 0.5kg of foaming cross-linking aid and 0.2kg of stearic acid into an internal mixer, stirring and mixing uniformly, adding 20kg of chlorinated paraffin and 13kg of naphthenic oil, continuing stirring and mixing uniformly, adding 15kg of butadiene-acrylonitrile rubber extruded into sheets in S1, stirring and mixing uniformly to form mixed rubber, and discharging.
S3, primary open mixing, which comprises the following steps:
pouring the mixed glue into two rollers of an open mill, and controlling the roller spacing of the two rollers to be 4mm, so that the thickness of the blank extruded into the sheet is about 4 mm.
S4, mixing and stirring, specifically comprising the following steps:
adding the extruded sheet blank of S3 into an internal mixer, stirring and mixing, gradually raising the internal mixing temperature, adding 6kg of foaming agent when the temperature reaches 105 ℃, continuously stirring and uniformly mixing to form a mixture, and then carrying out discharging operation.
S5, secondary open mixing, which comprises the following steps:
and (3) pouring the mixture which is stirred and mixed uniformly in the S4 into two rollers of an open mill, and controlling the roller distance of the two rollers to be 40mm so that the thickness of the mixture extruded into a sheet is about 40 mm. The mixture extruded into tablets was cut into pieces having a length of about 1m, and the pieces were weighed as needed.
S6, foaming, specifically comprising the following steps:
and (3) adding the weighed sheet materials in the S5 into a die of an oil pressure foaming machine for foaming, controlling the temperature of die pressing foaming to be 170 ℃, controlling the time of die pressing foaming to be 40min, opening the die after foaming is finished, taking out the foaming body, and cooling to obtain the nitrile rubber.
Example 3
The nitrile rubber comprises the following components in parts by mass:
20kg of nitrile rubber; 12kg of chlorinated paraffin; 10kg of naphthenic oil; carbon black N55012 kg; 30kg of polyvinyl chloride; 20kg of calcium carbonate; 7kg of foaming agent; 0.6kg of cross-linking agent DCP; 0.7kg of foaming crosslinking auxiliary agent; stearic acid 0.4 kg.
In this example, the blowing agent was azodimethylamide available from Jiangsu Soppe chemical company Limited under the designation DN 10.
In this example, the foaming crosslinking aid is zinc oxide.
The preparation method of the nitrile rubber comprises the following steps:
s1, separating the glue, which is specifically as follows:
pouring 20kg of nitrile rubber into two rollers of an open mill, controlling the temperature of the two rollers to be 60 ℃, controlling the roller spacing of the two rollers to be 2mm, enabling the thickness of the extruded sheet of nitrile rubber to be about 2mm, putting the extruded sheet of nitrile rubber into the two rollers of the open mill again, carrying out thin-passing treatment for 2 times, and discharging for later use.
S2, mixing the rubber, specifically as follows:
adding carbon black N55012 kg, 30kg of polyvinyl chloride, 20kg of calcium carbonate, 0.6kg of crosslinking agent DCP, 0.7kg of foaming crosslinking aid and 0.4kg of stearic acid into an internal mixer, pressing a pressure cover downwards to seal a feeding port, simultaneously preventing the pressure cover from contacting with raw materials, idling the internal mixer for 25s, and then stirring.
After the raw materials are stirred and uniformly mixed, stopping stirring, lifting the pressurizing cover, adding 12kg of chlorinated paraffin and 10kg of naphthenic oil, pressing the pressurizing cover downwards to seal the feeding port, simultaneously enabling the pressurizing cover not to be in contact with the raw materials, enabling the internal mixer to idle for 30S, lifting the pressurizing cover again, adding 20kg of butadiene-acrylonitrile rubber extruded into sheets in S1 to form mixed rubber, pressing the pressurizing cover downwards to enable the pressurizing cover to be abutted against the mixed rubber, stirring the mixed rubber, and simultaneously gradually raising the temperature. When the temperature reaches 110 ℃, partially lifting the pressurizing cover to ensure that the pressurizing cover does not contact with the mixed glue while sealing the feed inlet, and after cleaning the periphery of the pressurizing cover, downwards pressing the pressurizing cover to ensure that the pressurizing cover is abutted against the mixed glue and continuously stirring. After that, when the temperature rises by 3 ℃, the pressurizing cover is firstly lifted and the periphery of the pressurizing cover is cleaned, then the pressurizing cover is completely lifted, so that the feeding hole is opened, and the mixed glue is stirred and overturned once. When the temperature reaches 145 ℃, the mixed glue is discharged.
S3, primary open mixing, which comprises the following steps:
pouring the mixed glue into two rollers of an open mill with the roller diameter of 18 inches, and controlling the roller distance of the two rollers to be 1.5mm, so that the thickness of a blank formed by extruding the mixed glue into a sheet is about 1.5 mm; the stock discharged from the open mill having a roll diameter of 18 inches was pulled into two rolls of an open mill having a roll diameter of 16 inches, and the roll gap of the open mill having a roll diameter of 16 inches was controlled to be 1mm, so that the thickness of the finally discharged stock was about 1 mm.
S4, mixing and stirring, specifically comprising the following steps:
adding the blank extruded into the sheet by S3 into an internal mixer, pressing a pressurizing cover downwards to enable the pressurizing cover to be in contact with the blank, stirring and mixing the blank, simultaneously gradually raising the internal mixing temperature, partially lifting the pressurizing cover firstly when the temperature reaches 95 ℃ to enable the pressurizing cover to be separated from the blank, cleaning the periphery of the pressurizing cover, completely lifting the pressurizing cover to enable a feed inlet to be opened, adding 6kg of foaming agent, then pressing the pressurizing cover downwards to enable the pressurizing cover to be abutted against the blank, and continuing to stir the blank. After that, when the temperature rises by 3 ℃, the pressurizing cover is firstly lifted and the periphery of the pressurizing cover is cleaned, then the pressurizing cover is completely lifted, so that the feed port is opened, and the blank is stirred and turned over once. After being stirred evenly, a mixture is formed. When the temperature reaches 120 ℃, the discharging operation of the mixture is carried out.
S5, secondary open mixing, which comprises the following steps:
pouring the mixture stirred and uniformly mixed by the S4 into two rollers of an open mill with the roller diameter of 18 inches, and controlling the roller spacing of the two rollers to be 1.5mm, so that the thickness of the mixture extruded into a sheet is about 1.5 mm; the sheet-like mixture discharged from the open mill having a roll diameter of 18 inches was pulled into two rolls of the open mill having a roll diameter of 16 inches, and the roll gap of the open mill having a roll diameter of 16 inches was controlled to be 25mm, so that the thickness of the sheet-like mixture finally discharged was about 25 mm. The sheet mix discharged from the 16-inch mill was cut into pieces having a length of about 1m, and the pieces were weighed as needed.
S6, foaming, specifically comprising the following steps:
and (3) adding the weighed sheet materials in the S5 into a die of an oil pressure foaming machine for foaming, controlling the temperature of die pressing foaming to be 150 ℃, controlling the time of die pressing foaming to be 60min, opening the die after foaming is finished, taking out the foaming body, and cooling to obtain the nitrile rubber.
Example 4
The nitrile rubber comprises the following components in parts by mass:
13kg of nitrile rubber; 16kg of chlorinated paraffin; 15kg of naphthenic oil; carbon black N5509 kg; 40kg of polyvinyl chloride; 18kg of calcium carbonate; 8kg of foaming agent; crosslinking agent DCP0.8kg; 0.9kg of foaming crosslinking auxiliary agent; stearic acid 0.5 kg.
In this example, the blowing agent was azodimethylamide available from Jiangsu Soppe chemical company Limited under the designation DN 10.
In this example, the foaming crosslinking aid is zinc oxide.
The preparation method of the nitrile rubber comprises the following steps:
s1, separating the glue, which is specifically as follows:
pouring 13kg of nitrile rubber into two rollers of an open mill, controlling the temperature of the two rollers to be 65 ℃, controlling the roller spacing of the two rollers to be 3.5mm, enabling the thickness of the extruded sheet of nitrile rubber to be about 3.5mm, putting the extruded sheet of nitrile rubber into the two rollers of the open mill again, carrying out thin-pass treatment for 3 times, and discharging for later use.
S2, mixing the rubber, specifically as follows:
adding carbon black N5509 kg, 40kg of polyvinyl chloride, 18kg of calcium carbonate, 0.8kg of crosslinking agent DCP, 0.9kg of foaming crosslinking assistant and 0.5kg of stearic acid into an internal mixer, pressing down a pressure cover to seal a feeding port, simultaneously preventing the pressure cover from contacting with raw materials, idling the internal mixer for 30s, and then stirring.
After the raw materials are stirred and uniformly mixed, stopping stirring, lifting the pressurizing cover, adding 16kg of chlorinated paraffin and 15kg of naphthenic oil, pressing the pressurizing cover downwards to seal the feeding port, simultaneously enabling the pressurizing cover not to be in contact with the raw materials, enabling the internal mixer to idle for 35S, lifting the pressurizing cover again, adding 13kg of butadiene-acrylonitrile rubber extruded into sheets in S1 to form mixed rubber, pressing the pressurizing cover downwards to enable the pressurizing cover to be abutted against the mixed rubber, stirring the mixed rubber, and simultaneously gradually raising the temperature. When the temperature reaches 115 ℃, partially lifting the pressurizing cover to ensure that the pressurizing cover does not contact with the mixed glue while closing the feed inlet, and after cleaning the periphery of the pressurizing cover, downwards pressing the pressurizing cover to ensure that the pressurizing cover is abutted against the mixed glue and continuously stirring. After that, when the temperature rises by 5 ℃, the pressurizing cover is firstly lifted and the periphery of the pressurizing cover is cleaned, then the pressurizing cover is completely lifted, so that the feeding hole is opened, and the mixed glue is stirred and overturned once. When the temperature reaches 150 ℃, the mixed glue is discharged.
S3, primary open mixing, which comprises the following steps:
pouring the mixed glue into two rollers of an open mill with the roller diameter of 18 inches, and controlling the roller distance of the two rollers to be 1mm, so that the thickness of a blank formed by extruding the mixed glue into a sheet is about 1 mm; the stock discharged from the open mill having a roll diameter of 18 inches was pulled into two rolls of an open mill having a roll diameter of 16 inches, and the roll gap of the open mill having a roll diameter of 16 inches was controlled to be 2mm, so that the thickness of the finally discharged stock was about 2 mm.
S4, mixing and stirring, specifically comprising the following steps:
adding the blank extruded into the sheet by S3 into an internal mixer, pressing a pressurizing cover downwards to enable the pressurizing cover to be in contact with the blank, stirring and mixing the blank, simultaneously gradually raising the internal mixing temperature, partially lifting the pressurizing cover firstly when the temperature reaches 100 ℃ to enable the pressurizing cover to be separated from the blank, cleaning the periphery of the pressurizing cover, completely lifting the pressurizing cover to enable a feed inlet to be opened, adding 8kg of foaming agent, then pressing the pressurizing cover downwards to enable the pressurizing cover to be abutted against the blank, and continuously stirring the blank. After that, when the temperature rises by 4 ℃, the pressurizing cover is firstly lifted and the periphery of the pressurizing cover is cleaned, then the pressurizing cover is completely lifted, so that the feed port is opened, and the blank is stirred and turned over once. After being stirred evenly, a mixture is formed. When the temperature reaches 130 ℃, discharging the mixture.
S5, secondary open mixing, which comprises the following steps:
pouring the mixture stirred and uniformly mixed by the S4 into two rollers of an open mill with the roller diameter of 18 inches, and controlling the roller spacing of the two rollers to be 1.5mm, so that the thickness of the mixture extruded into a sheet is about 1.5 mm; the sheet-like mixture discharged from the open mill having a roll diameter of 18 inches was pulled into two rolls of the open mill having a roll diameter of 16 inches, and the roll gap of the open mill having a roll diameter of 16 inches was controlled to be 30mm, so that the thickness of the sheet-like mixture finally discharged was about 30 mm. The sheet mix discharged from the 16-inch mill was cut into pieces having a length of about 1m, and the pieces were weighed as needed.
S6, foaming, specifically comprising the following steps:
and (3) adding the weighed sheet materials in the S5 into a die of an oil pressure foaming machine for foaming, controlling the temperature of die pressing foaming to be 158 ℃, controlling the time of die pressing foaming to be 53min, after foaming is finished, opening the die, taking out the foaming body, and cooling to obtain the nitrile rubber.
Example 5
The nitrile rubber comprises the following components in parts by mass:
18kg of nitrile rubber; 18kg of chlorinated paraffin; 20kg of naphthenic oil; carbon black N5506 kg; 35kg of polyvinyl chloride; 13kg of calcium carbonate; 3kg of foaming agent; 0.5kg of crosslinking agent DCP; 1kg of foaming crosslinking auxiliary agent; stearic acid 0.3 kg.
In this example, the blowing agent was azodimethylamide available from Jiangsu Soppe chemical company Limited under the designation DN 10.
In this example, the foaming crosslinking aid is zinc oxide.
The preparation method of the nitrile rubber comprises the following steps:
s1, separating the glue, which is specifically as follows:
pouring 18kg of nitrile rubber into two rollers of an open mill, controlling the temperature of the two rollers to be 70 ℃, controlling the roller spacing of the two rollers to be 5mm, enabling the thickness of the extruded sheet of nitrile rubber to be about 5mm, putting the extruded sheet of nitrile rubber into the two rollers of the open mill again, carrying out thin-passing treatment for 4 times, and discharging for later use.
S2, mixing the rubber, specifically as follows:
adding carbon black N5506 kg, 35kg of polyvinyl chloride, 13kg of calcium carbonate, 0.5kg of crosslinking agent DCP, 1kg of foaming crosslinking aid and 0.3kg of stearic acid into an internal mixer, pressing a pressure cover downwards to seal a feeding port, simultaneously enabling the pressure cover not to contact with raw materials, and stirring after the internal mixer idles for 35 s.
After the raw materials are stirred and uniformly mixed, stopping stirring, lifting the pressurizing cover, adding 18kg of chlorinated paraffin and 20kg of naphthenic oil, pressing the pressurizing cover downwards to seal the feeding port, simultaneously enabling the pressurizing cover not to be in contact with the raw materials, enabling the internal mixer to idle for 25S, lifting the pressurizing cover again, adding 18kg of butadiene-acrylonitrile rubber extruded into sheets in S1 to form mixed rubber, pressing the pressurizing cover downwards to enable the pressurizing cover to be abutted against the mixed rubber, stirring the mixed rubber, and simultaneously gradually raising the temperature. When the temperature reaches 120 ℃, partially lifting the pressurizing cover to ensure that the pressurizing cover does not contact with the mixed glue while sealing the feed inlet, and after cleaning the periphery of the pressurizing cover, downwards pressing the pressurizing cover to ensure that the pressurizing cover is abutted against the mixed glue and continuously stirring. After that, when the temperature rises by 3 ℃, the pressurizing cover is firstly lifted and the periphery of the pressurizing cover is cleaned, then the pressurizing cover is completely lifted, so that the feeding hole is opened, and the mixed glue is stirred and overturned once. When the temperature reaches 155 ℃, the mixed glue is discharged.
S3, primary open mixing, which comprises the following steps:
pouring the mixed glue into two rollers of an open mill with the roller diameter of 18 inches, and controlling the roller distance of the two rollers to be 1.5mm, so that the thickness of a blank formed by extruding the mixed glue into a sheet is about 1.5 mm; the stock discharged from the open mill having a roll diameter of 18 inches was pulled into two rolls of an open mill having a roll diameter of 16 inches, and the roll gap of the open mill having a roll diameter of 16 inches was controlled to be 3mm, so that the thickness of the finally discharged stock was about 3 mm.
S4, mixing and stirring, specifically comprising the following steps:
adding the blank extruded into the sheet by S3 into an internal mixer, pressing a pressurizing cover downwards to enable the pressurizing cover to be in contact with the blank, stirring and mixing the blank, simultaneously gradually raising the internal mixing temperature, partially lifting the pressurizing cover firstly when the temperature reaches 105 ℃ to enable the pressurizing cover to be separated from the blank, cleaning the periphery of the pressurizing cover, completely lifting the pressurizing cover to enable a feed inlet to be opened, adding 3kg of foaming agent, then pressing the pressurizing cover downwards to enable the pressurizing cover to be abutted against the blank, and continuing to stir the blank. After that, when the temperature rises by 3 ℃, the pressurizing cover is firstly lifted and the periphery of the pressurizing cover is cleaned, then the pressurizing cover is completely lifted, so that the feed port is opened, and the blank is stirred and turned over once. After being stirred evenly, a mixture is formed. When the temperature reaches 140 ℃, the discharging operation of the mixture is carried out.
S5, secondary open mixing, which comprises the following steps:
pouring the mixture stirred and uniformly mixed by the S4 into two rollers of an open mill with the roller diameter of 18 inches, and controlling the roller spacing of the two rollers to be 1.5mm, so that the thickness of the mixture extruded into a sheet is about 1.5 mm; the sheet-like mixture discharged from the open mill having a roll diameter of 18 inches was pulled into two rolls of the open mill having a roll diameter of 16 inches, and the roll gap of the open mill having a roll diameter of 16 inches was controlled to 35mm, so that the thickness of the sheet-like mixture finally discharged was about 35 mm. The sheet mix discharged from the 16-inch mill was cut into pieces having a length of about 1m, and the pieces were weighed as needed.
S6, foaming, specifically comprising the following steps:
and (3) adding the weighed sheet materials in the S5 into a die of an oil pressure foaming machine for foaming, controlling the temperature of die pressing foaming to be 165 ℃ and the time of die pressing foaming to be 45min, opening the die after foaming is finished, taking out the foaming body, and cooling to obtain the nitrile butadiene rubber.
Comparative example 1
Example 1 of "a polysiloxane-modified nitrile rubber, a synthetic method and preparation of vulcanized rubber thereof" in chinese patent document No. CN102516558B was used as a comparative example.
Experiment 1
The nitrile rubbers obtained in the above examples were tested for their brittleness temperature (. degree. C.) according to GB/T1682-1994, Single sample method for determination of Low temperature brittleness of vulcanizates.
Experiment 2
The cold resistance coefficient under-55 ℃ of the nitrile rubber prepared in the above examples was measured according to GB/T6034-1985 "determination of Cold resistance coefficient under compression of vulcanized rubber".
Experiment 3
The nitrile rubbers obtained in the above examples were tested for compression set (%) according to GB/T1683-2018 method for determining the compression set at constant set of vulcanized rubber.
The above test data are shown in Table 1.
TABLE 1
| Brittleness temperature (. degree.C.) | Cold resistance coefficient under compression | Compression set (%) | |
| Example 1 | -77 | 0.481 | 6 |
| Example 2 | -76 | 0.472 | 6 |
| Example 3 | -85 | 0.641 | 3 |
| Example 4 | -84 | 0.652 | 2 |
| Example 5 | -85 | 0.643 | 2 |
| Comparative example 1 | -71 | 0.361 | 13 |
Comparing the data of examples 1-5 with that of comparative example 1 in Table 1, it can be seen that the nitrile rubbers prepared by the component proportion and the preparation method of the present invention are used in examples 1-5, the nitrile rubber prepared by the prior art is used in comparative example 1, the brittle temperature of examples 1-5 is much lower than that of comparative example 1, the cold resistance coefficient under compression is much higher than that of comparative example 1 in examples 1-5, and the compression set rate of examples 1-5 is much lower than that of comparative example 1, i.e. the rebound resilience and the low temperature resistance of the nitrile rubbers prepared in examples 1-5 are better than those of comparative example 1, which shows that the preparation of the nitrile rubbers by the component proportion and the preparation method of the present invention is beneficial to improving the uniformity of the cells of the nitrile rubbers, enhancing the rebound resilience of the nitrile rubbers, and making the rebound resilience of the nitrile rubbers not easily affected by low temperature, the low-temperature resistance of the nitrile rubber is enhanced, and the nitrile rubber has a wider application range.
As can be seen from the comparison of the data in Table 1 between examples 1-2 and examples 3-5, examples 1-2 used urea resin BK as the blowing agent, silica as the foaming crosslinking aid, examples 3-5 used azodicarbonamide as the blowing agent, and zinc oxide as the foaming crosslinking aid, and examples 1-2 lacked the operation of stirring and inverting the mixture in the internal mixer once per 3 ℃ to 5 ℃ rise in the temperature during the internal mixing process as compared with examples 3-5, while examples 1-2 and examples 3-5 had differences in the internal mixing temperature and time, whereas examples 3-5 had brittle temperatures lower than examples 1-2 and examples 3-5 had compression cold resistance higher than examples 1-2, the compression set of examples 3-5 is lower than that of examples 1-2, i.e., the resilience and low temperature resistance of examples 3-5 are better than those of examples 1-2, which shows that azodicarbonamide is adopted as a foaming agent, zinc oxide is adopted as a foaming crosslinking assistant, azodicarbonamide has higher decomposition temperature and is not easy to decompose in advance in banburying, and meanwhile, the zinc oxide is added to facilitate the reduction of the decomposition temperature of azodicarbonamide and the reduction of the decomposition temperature of the foaming agent, thereby facilitating the foaming initiation of the foaming agent, facilitating the control of the foaming process of the nitrile rubber after the crosslinking process, enabling the crosslinking foaming and foaming of the nitrile rubber to be more sufficient, facilitating the crosslinking of the nitrile rubber to form a network structure, and simultaneously enabling the foam cells of the prepared nitrile rubber to be more uniform, the rebound resilience and the heat preservation of the nitrile rubber are improved, the rebound resilience of the nitrile rubber is not easily influenced by low temperature, the low temperature resistance of the nitrile rubber is enhanced, and the application range of the nitrile rubber is wider; through the in-process that the temperature at banburying process rises, the temperature is every 3 ℃ -5 ℃ that rises, the temperature and the time of stirring in the upset banbury mixer are once and through controlling the banburying, it is more even to be favorable to each component mixing dispersion of butadiene acrylonitrile rubber, thereby be favorable to abundant foaming and abundant crosslinking of butadiene acrylonitrile rubber, make butadiene acrylonitrile rubber's resilience improve, make butadiene acrylonitrile rubber's resilience be difficult to receive microthermal influence simultaneously, be favorable to improving butadiene acrylonitrile rubber's low temperature resistance ability, make butadiene acrylonitrile rubber's application scope wider.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (6)
1. A nitrile rubber, which is characterized in that: the paint comprises the following components in parts by mass:
10-20 parts of nitrile rubber;
12-20 parts of chlorinated paraffin;
10-20 parts of naphthenic oil;
carbon black N5506-12 shares;
30-40 parts of polyvinyl chloride;
10-20 parts of calcium carbonate;
3-10 parts of a foaming agent;
0.5-0.8 part of DCP serving as a crosslinking agent;
0.5-1 part of foaming crosslinking auxiliary agent;
0.2-0.5 part of stearic acid;
the foaming agent is azodicarbonamide;
the foaming crosslinking auxiliary agent is zinc oxide;
the preparation method of the nitrile rubber comprises the following steps:
s1, glue separation: extruding nitrile rubber into sheets;
s2, mixing rubber: firstly, mixing and stirring polyvinyl chloride, carbon black, calcium carbonate, a crosslinking agent DCP, a foaming crosslinking aid and stearic acid uniformly, then adding chlorinated paraffin and naphthenic oil, stirring and mixing uniformly, then adding S1 to extrude into sheets of nitrile rubber, mixing uniformly to form mixed rubber, and discharging;
s3, primary open mixing: stirring and compacting the mixed glue, and extruding into sheets to form blanks;
s4, mixing and stirring: carrying out banburying on the blank formed by the S3, gradually raising the banburying temperature, adding a foaming agent when the temperature reaches 95-105 ℃, uniformly stirring and mixing to form a mixture, and discharging;
s5, secondary open mixing: extruding the mixture of S4 into sheets to form sheet materials, and controlling the thickness of the sheet materials to be 25-35 mm;
s6, foaming: adding the sheet material into a mold for foaming, controlling the foaming temperature to be 150-165 ℃, controlling the foaming time to be 45-60 min, opening the mold, cooling, and taking out the foaming body to obtain the nitrile rubber;
in the step S2, the temperature is gradually increased after the nitrile rubber extruded into the sheet is added, when the temperature reaches 110-120 ℃, the temperature is increased by 3-5 ℃ every time the temperature is increased, the mixed rubber is stirred and overturned once, and when the temperature reaches 145-155 ℃, the mixed rubber discharging operation is carried out.
2. The nitrile rubber according to claim 1, characterized in that: in the step S1, the temperature of the extruded sheet is controlled to be 60-70 ℃.
3. The nitrile rubber according to claim 1, characterized in that: in the step S1, the nitrile rubber is subjected to thin-pass treatment for 2 to 4 times and then discharged.
4. The nitrile rubber according to any of claims 1 to 3, characterized in that: in the step S1, the thickness of the nitrile rubber extruded into the sheet is controlled to be 2mm-5 mm.
5. The nitrile rubber according to any of claims 1 to 3, characterized in that: in the step S3, the thickness of the extruded sheet billet is controlled to be 1mm-3 mm.
6. The nitrile rubber according to any of claims 1 to 3, characterized in that: in the step S4, after the foaming agent is added, the mixture is stirred and overturned once when the temperature rises to 3-5 ℃, and when the temperature reaches 120-140 ℃, the discharging operation is carried out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910382589.9A CN110066481B (en) | 2019-05-09 | 2019-05-09 | Nitrile rubber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910382589.9A CN110066481B (en) | 2019-05-09 | 2019-05-09 | Nitrile rubber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110066481A CN110066481A (en) | 2019-07-30 |
| CN110066481B true CN110066481B (en) | 2022-01-11 |
Family
ID=67370367
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910382589.9A Active CN110066481B (en) | 2019-05-09 | 2019-05-09 | Nitrile rubber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110066481B (en) |
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110066481A (en) | 2019-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101633753B (en) | Neoprene closed cell foamed material and preparation method thereof | |
| CN101255242B (en) | Butadiene styrene rubber foaming plate and preparation thereof | |
| CN101392076B (en) | Duprene rubber foamed sheet and preparation method thereof | |
| CN102532725A (en) | Activated resol cure rubber composition | |
| CN110028726A (en) | A kind of gross porosity EVA moulded from foam material and preparation method thereof | |
| CN111675858A (en) | Formula and preparation method of corrosion-resistant rubber material | |
| CN107841020B (en) | Crosslinked polyethylene foam material and preparation method thereof | |
| CN102199322A (en) | Irradiation cross-linked heat resistant flame-retardant rubber-plastic compound conductive foam and manufacturing method thereof | |
| CN110066481B (en) | Nitrile rubber and preparation method thereof | |
| CN111548570B (en) | High-performance ethylene propylene rubber sealing gasket, and preparation method and application thereof | |
| CN102219946B (en) | Low-halogen environment-friendly chloroprene rubber (CR) closed-cell foam material and preparation method thereof | |
| WO2022001557A1 (en) | High elastic nylon and preparation method therefor | |
| CN105037851A (en) | Butadiene styrene rubber, natural rubber and acrylonitrile-butadiene rubber combined obturator secondary foaming material and preparing method thereof | |
| CN109942975A (en) | Gasket and its feedstock composition, production method | |
| CN114230877A (en) | Blending system and mixing process of isoprene rubber and brominated butyl rubber | |
| CN110713664A (en) | Preparation method of tire curing bladder | |
| WO2019095787A1 (en) | Nitrile rubber for pneumatic nail gun cushion and preparation method therefor | |
| CN109648725B (en) | Method for producing rubber compound | |
| CN114015166A (en) | EPDM rubber foaming material and application | |
| CN105175903B (en) | A kind of modified rubber addition auxiliary agent and preparation method thereof | |
| CN111873209A (en) | Production process of low-temperature-resistant silicone rubber | |
| CN109385017A (en) | Compounded rubber and preparation method thereof and its application in EVA foaming | |
| CN103642080A (en) | Natural rubber sponge with high compressive load retention rate and preparation method thereof | |
| CN109485942A (en) | A kind of preparation method of nitrile rubber | |
| CN116120622B (en) | Polypropylene foaming bead, preparation method and molded part thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |