CN110498881A - A kind of method of high intensity carboxyl type acrylic rubber - Google Patents
A kind of method of high intensity carboxyl type acrylic rubber Download PDFInfo
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- CN110498881A CN110498881A CN201910639235.8A CN201910639235A CN110498881A CN 110498881 A CN110498881 A CN 110498881A CN 201910639235 A CN201910639235 A CN 201910639235A CN 110498881 A CN110498881 A CN 110498881A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- Chemical Kinetics & Catalysis (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of methods of high-intensitive carboxylic acid type acrylic rubber, comprising the following steps: step S1, determines raw material ratio；Step S2, prepared by small powder；Step S3, raw material premix；Step S4, emulsion polymerization；Step S5, demulsification cohesion；Step S6, glue is washed；Step S7, it dries；Step S8, it packs；The beneficial effects of the invention are as follows, acrylic rubber according to this method manufacture is due to using carboxyl to have excellent permanent compression set as hinge monomer, and it joined with high-intensitive modified monomer, product strength is up to 18MPa or so after modified monomer accounts for polymerized monomer 15% (methyl acrylate: propylene is fine=1:1) polymerization, and prepared acrylic rubber is suitable in the mechanical sealing member environment that intensity requirement is high and compression set is small.
Description
Technical field
The present invention relates to technical field of rubber preparation, especially a kind of method of high-intensitive carboxyl type acrylic rubber.
Background technique
Acrylic rubber is a kind of synthetic rubber made of being copolymerized using acrylate as principal monomer, has resistance to height
The properties such as temperature, oil resistant, ozone-resistant and UV resistant irradiation, are a kind of heat-resisting, oil resistant specific rubbers, are mainly used as automobile
With various heat-resisting oil-resistant seal rings, liner and the oil sealing of locomotive, the comonomer of acrylic rubber can be divided into main monomer, low temperature
Oil resistant monomer and cure site monomer etc., common main monomer have methyl acrylate, ethyl acrylate, butyl acrylate and propylene
Acid -2- ethylhexyl etc.；
And being showing improvement or progress day by day with science and technology, people start to be more reasonably utilized tool, need in the process a large amount of
Using rubber product, and existing rubber is in the environment of leakproofness, since its intensity is not high, the ability of pressure-resistant compression permanent deformation
Difference can generate a large amount of abrasions due to mechanical loss, bring very big workload to later maintenance and maintenance, and can bring not
Necessary supplies consumption, causes cost increase, in consideration of it, furtheing investigate regarding to the issue above, there is this case generation then.
Summary of the invention
The purpose of the present invention is to solve the above problems, devise a kind of side of high-intensitive carboxyl type acrylic rubber
Method solves existing rubber in the environment of leakproofness, and since its intensity is not high, the ability of pressure-resistant compression permanent deformation is poor, meeting
A large amount of abrasions are generated due to mechanical loss, to later maintenance and maintenance bring very big workload, and can bring it is unnecessary
Supplies consumption, the problem of causing cost increase.
Above-mentioned purpose is realized the technical solution of the present invention is as follows: a kind of method of high intensity carboxyl type acrylic rubber, packet
It includes following steps: step S1, determining raw material ratio；Step S2, prepared by small powder；Step S3, raw material premix；Step S4, lotion
Polymerization；Step S5, demulsification cohesion；Step S6, glue is washed；Step S7, it dries；Step S8, it packs；
Step S1: main monomer chooses butyl acrylate and ethyl acrylate (the two accounting 70%-85%), acrylic acid first
Ester or acrylonitrile are as enhancing monomer (accounting 10%-15%), one of acrylic acid, maleic acid and itaconic acid or two kinds
As cross-linking monomer (10%-5%)；
Step S2: configuration small powder, small powder includes: molecular weight regulator, polymerization inhibitor and demulsifier；
Step S3: main monomer and cross-linking monomer being added in premix kettle and is configured to premix emulsion, and the time about 30 minutes；
Step S4: being added water in a kettle, and the emulsifier (lauryl sodium sulfate+OP-10) of 1%-6% is then added
Lotion is made in stirring 30 minutes.The premix raw material premixed in kettle is added in lotion again, emulsification, mixing time is sufficiently stirred
30min.Keep temperature 30 --- 90 degree, initiator (cumyl hydroperoxide) is added into lotion, reaction starts.
Step S5: after reacting 1~8 hour in step s 4, material is arranged to collection surface, polymerization inhibitor is added and stirs 30min
Demulsifier is added, is demulsified to obtain target product under the conditions of 70~75 DEG C；
Step S6: the obtained carboxyl type acrylic rubber in step S5 is carried out sufficiently under 45~82 DEG C of water temperature
Washing；
Step S7: the carboxyl type acrylic rubber after washing is dried in the environment of 70~120 DEG C of temperature；
Step S8: the carboxyl type acrylic rubber after drying is subjected to cutting packaging.
Methyl methacrylate accounting in the step S1 is 5%~10%, acrylonitrile accounting is 5%~10%.
A length of half an hour when stirring in the step S3.
After initiator is added in the step S4, select the thiol solution of concentration 1.05%~1.1% as molecular weight tune
Section agent is added in polymerized emulsion.
Polymerization inhibitor selects hydroquinone in the step S5, and its additive capacity is a ten thousandth as mass fraction.
It is 1% sodium chloride solution that the demulsifier added in the step S5, which selects mass fraction,.
It is 70~80 DEG C that temperature of reaction kettle is kept in the step S4 polymerization process, and the reaction time is 2 hours.
Water temperature in the step S6 is set as 50~60 DEG C.
Drying temperature in the step S7 is set as 100~110 DEG C.
The present invention provides a kind of methods of high-intensitive carboxyl type acrylic rubber, the acrylic acid according to this method manufacture
Ester rubber, by the way that enhancing monomer and carboxylic acid type cross-linking monomer is added in rubber, due to its carboxyl presence thus have it is good
Good permanent compression set, and since the effect of enhancing monomer has the higher-strength greater than 15MPa, prepared acrylate
Rubber is suitable in the mechanical sealing member environment that intensity requirement is high and compression set is small.
Specific embodiment
The present invention is specifically described below, a kind of method of high intensity carboxyl type acrylic rubber, including following
Step: raw material ratio step S1, is determined；Step S2, prepared by small powder；Step S3, raw material premix；Step S4, emulsion polymerization；Step
Rapid S5, demulsification cohesion；Step S6, glue is washed；Step S7, it dries；Step S8, it packs；Step S1: main monomer chooses butyl acrylate
And ethyl acrylate (the two accounting 70%-85%), methyl acrylate or acrylonitrile are as enhancing monomer (accounting 10%-
15%), one of acrylic acid, maleic acid and itaconic acid or two kinds of conducts cross-linking monomer (10%-5%)；Step S2: match
Small powder is set, small powder includes: molecular weight regulator, polymerization inhibitor and demulsifier；Step S3: in a kettle be added main monomer and
Cross-linking monomer is simultaneously configured to premix emulsion；Step S4: being added water in a kettle, and the emulsifier (12 of 1%-6% is then added
Sodium alkyl sulfate+OP-10) stirring 30 minutes, lotion is made.The premix raw material premixed in kettle is added in lotion again and is sufficiently stirred
Emulsification, mixing time 30min.Keep temperature 30 --- 90 degree, initiator (cumyl hydroperoxide) is added into lotion, instead
It should start.Step S5: after reacting 1~8 hour in step s 4, material being arranged to collection surface, and polymerization inhibitor stirring 30min is added and adds
Enter demulsifier, is demulsified to obtain target product under the conditions of 70~75 DEG C；Step S6: by the obtained carboxyl type in step S5
Acrylic rubber is sufficiently washed under 45~82 DEG C of water temperature；Step S7: to the carboxyl type acrylate rubber after washing
Glue is dried in the environment of 70~110 DEG C of temperature；Step S8: the carboxyl type acrylic rubber after drying is cut
Packaging；Methyl methacrylate accounting in the step S1 is 5%~10%, acrylonitrile accounting is 5%~10%；The step
A length of half an hour when stirring in rapid S3；After initiator is added in the step S4, the mercaptan of concentration 1.05%~1.1% is selected
Solution is added in polymerized emulsion as molecular weight regulator；Polymerization inhibitor selects hydroquinone in the step S5, and it is added
Dosage is a ten thousandth as mass fraction；It is 1% sodium chloride that the demulsifier added in the step S5, which selects mass fraction,
Solution；It is 70~80 DEG C that temperature of reaction kettle is kept in the step S4 polymerization process, and the reaction time is 2 hours；The step S6
In water temperature be set as 50~60 DEG C；Drying temperature in the step S7 is set as 100~110 DEG C.
The characteristics of the present embodiment is, comprising the following steps: step S1, determines raw material ratio；Step S2, small powder system
It is standby；Step S3, raw material premix；Step S4, emulsion polymerization；Step S5, demulsification cohesion；Step S6, glue is washed；Step S7, it dries；Step
Rapid S8, packaging；Step S1: main monomer chooses butyl acrylate and ethyl acrylate (the two accounting 70%-85%), acrylic acid
Methyl esters or acrylonitrile are as enhancing monomer (accounting 10%-15%), one of acrylic acid, maleic acid and itaconic acid or two
Kind is used as cross-linking monomer (10%-5%)；Step S2: configuration small powder, small powder includes: molecular weight regulator, polymerization inhibitor and demulsification
Agent；Step S3: main monomer and cross-linking monomer are added in a kettle and is configured to premix emulsion；Step S4: in a kettle
Water is added, the emulsifier (lauryl sodium sulfate+OP-10) that 1%-6% is then added stirs 30 minutes, and lotion is made.Again will
Premix raw material in premix kettle, which is added in lotion, is sufficiently stirred emulsification, mixing time 30min.Keep temperature 30 --- 90 degree, to
Initiator (cumyl hydroperoxide) is added in lotion, reaction starts.Step S5: after reacting 1~8 hour in step s 4,
Material is arranged to collection surface, polymerization inhibitor stirring 30min is added, demulsifier is added, be demulsified to obtain mesh under the conditions of 70~75 DEG C
Mark product；Step S6: the obtained carboxyl type acrylic rubber in step S5 is carried out sufficiently under 45~82 DEG C of water temperature
Washing；Step S7: the carboxyl type acrylic rubber after washing is dried in the environment of 70~120 DEG C of temperature；Step
S8: the carboxyl type acrylic rubber after drying is subjected to cutting packaging；According to the acrylic rubber of this method manufacture, pass through
Enhancing monomer and carboxylic acid type cross-linking monomer is added in rubber, due to its carboxyl presence thus there is good permanent compression
Deformation, and since the effect of enhancing monomer has the higher-strength greater than 15MPa, prepared acrylic rubber is suitable for
In the mechanical sealing member environment that intensity requirement is high and compression set is small.
1, the preparation of high-intensitive carboxyl type acrylic rubber sample:
Embodiment 1: in the specific implementation process, in accordance with the following steps and proportion is operated:
(1) it premixes: by (methyl methacrylate 5% and the acrylonitrile 1%) as enhancing monomer, then plus (acrylic acid
Butyl ester and ethyl acrylate 75%), then 10% acrylic acid is chosen as cross-linking monomer, it is added in premix kettle and stirs 30 minutes
It is spare；
(2) small powder configures: mercaptan that 1.05%~1.1% concentration of molecular weight regulator is respectively configured, polymerization inhibitor are (very much
One of hydroquinone) and demulsifier 1% sodium chloride solution；
(3) polymerization reaction: being added water in a kettle under room temperature, 5% emulsifier (dodecyl sulphate is then added
Sodium+OP-10) and (two) in the molecular weight regulator that stirs evenly, stir 30 minutes, lotion be made.It will premix again pre- in kettle
Mixed raw material, which is added in lotion, is sufficiently stirred emulsification, and initiator is added in mixing time 30min, and initiator selects hydrop isopropyl
Benzole soln makes to start polymerization reaction in mixed emulsion, and heat of polymerization is warming up to 90 degree after discharging, keep the temperature 2 hours, reacted
At；
(4) it agglomerates: after polymerization reaction 2 hours, material being arranged to collection surface, it is broken that polymerization inhibitor stirring 30min addition is added
Emulsion is demulsified to obtain target product under the conditions of 70~75 DEG C, carries out carrying out under 50~60 DEG C of water temperatures respectively later more
It is secondary to wash glue；
(5) drying glue, packaging: carrying out air-dried at 100~110 DEG C, then carries out cutting packaging to rubber.
Embodiment 2: in the specific implementation process, in accordance with the following steps and proportion is operated:
(1) it premixes: by (methyl methacrylate 5% and the acrylonitrile 3%) as enhancing monomer, then plus (acrylic acid
Butyl ester and ethyl acrylate 75%), then 10% acrylic acid is chosen as cross-linking monomer, it is added in premix kettle and stirs 30 minutes
It is spare；
(2) small powder configures: mercaptan that 1.05%~1.1% concentration of molecular weight regulator is respectively configured, polymerization inhibitor are (very much
One of hydroquinone) and demulsifier 1% sodium chloride solution；
(3) polymerization reaction: being added water in a kettle under room temperature, 5% emulsifier (dodecyl sulphate is then added
Sodium+OP-10) and (two) in the molecular weight regulator that stirs evenly, stir 30 minutes, lotion be made.It will premix again pre- in kettle
Mixed raw material, which is added in lotion, is sufficiently stirred emulsification, and initiator is added in mixing time 30min, and initiator selects hydrop isopropyl
Benzole soln makes to start polymerization reaction in mixed emulsion, and heat of polymerization is warming up to 90 degree after discharging, keep the temperature 2 hours, reacted
At；
(4) it agglomerates: after polymerization reaction 2 hours, material being arranged to collection surface, it is broken that polymerization inhibitor stirring 30min addition is added
Emulsion is demulsified to obtain target product under the conditions of 70~75 DEG C, carries out carrying out under 50~60 DEG C of water temperatures respectively later more
It is secondary to wash glue；
(5) drying glue, packaging: carrying out air-dried at 100~110 DEG C, then carries out cutting packaging to rubber.
Embodiment 3: in the specific implementation process, in accordance with the following steps and proportion is operated:
(1) it premixes: by (methyl methacrylate 5% and the acrylonitrile 5%) as enhancing monomer, then plus (acrylic acid
Butyl ester and ethyl acrylate 75%), then 10% acrylic acid is chosen as cross-linking monomer, it is added in premix kettle and stirs 30 minutes
It is spare；
(2) small powder configures: mercaptan that 1.05%~1.1% concentration of molecular weight regulator is respectively configured, polymerization inhibitor are (very much
One of hydroquinone) and demulsifier 1% sodium chloride solution；
(3) polymerization reaction: being added water in a kettle under room temperature, 5% emulsifier (dodecyl sulphate is then added
Sodium+OP-10) and (two) in the molecular weight regulator that stirs evenly, stir 30 minutes, lotion be made.It will premix again pre- in kettle
Mixed raw material, which is added in lotion, is sufficiently stirred emulsification, and initiator is added in mixing time 30min, and initiator selects hydrop isopropyl
Benzole soln makes to start polymerization reaction in mixed emulsion, and heat of polymerization is warming up to 90 degree after discharging, keep the temperature 2 hours, reacted
At；
(4) it agglomerates: after polymerization reaction 2 hours, material being arranged to collection surface, it is broken that polymerization inhibitor stirring 30min addition is added
Emulsion is demulsified to obtain target product under the conditions of 70~75 DEG C, carries out carrying out under 50~60 DEG C of water temperatures respectively later more
It is secondary to wash glue；
(5) drying glue, packaging: carrying out air-dried at 100~110 DEG C, then carries out cutting packaging to rubber.
Embodiment 4: in the specific implementation process, in accordance with the following steps and proportion is operated:
(1) it premixes: by (methyl methacrylate 7% and the acrylonitrile 5%) as enhancing monomer, then plus (acrylic acid
Butyl ester and ethyl acrylate 75%), then 10% acrylic acid is chosen as cross-linking monomer, it is added in premix kettle and stirs 30 minutes
It is spare；
(2) small powder configures: mercaptan that 1.05%~1.1% concentration of molecular weight regulator is respectively configured, polymerization inhibitor are (very much
One of hydroquinone) and demulsifier 1% sodium chloride solution；
(3) polymerization reaction: being added water in a kettle under room temperature, 5% emulsifier (dodecyl sulphate is then added
Sodium+OP-10) and (two) in the molecular weight regulator that stirs evenly, stir 30 minutes, lotion be made.It will premix again pre- in kettle
Mixed raw material, which is added in lotion, is sufficiently stirred emulsification, and initiator is added in mixing time 30min, and initiator selects hydrop isopropyl
Benzole soln makes to start polymerization reaction in mixed emulsion, and heat of polymerization is warming up to 90 degree after discharging, keep the temperature 2 hours, reacted
At；
(4) it agglomerates: after polymerization reaction 2 hours, material being arranged to collection surface, it is broken that polymerization inhibitor stirring 30min addition is added
Emulsion is demulsified to obtain target product under the conditions of 70~75 DEG C, carries out carrying out under 50~60 DEG C of water temperatures respectively later more
It is secondary to wash glue；
(5) drying glue, packaging: carrying out air-dried at 100~110 DEG C, then carries out cutting packaging to rubber.
Embodiment 5: in the specific implementation process, in accordance with the following steps and proportion is operated:
(1) it premixes: by (methyl methacrylate 10% and the acrylonitrile 5%) as enhancing monomer, then plus (propylene
Acid butyl ester and ethyl acrylate 75%), then 10% acrylic acid is chosen as cross-linking monomer, it is added in premix kettle and stirs 30 points
Clock is spare；
(2) small powder configures: mercaptan that 1.05%~1.1% concentration of molecular weight regulator is respectively configured, polymerization inhibitor are (very much
One of hydroquinone) and demulsifier 1% sodium chloride solution；
(3) polymerization reaction: being added water in a kettle under room temperature, 5% emulsifier (dodecyl sulphate is then added
Sodium+OP-10) and (two) in the molecular weight regulator that stirs evenly, stir 30 minutes, lotion be made.It will premix again pre- in kettle
Mixed raw material, which is added in lotion, is sufficiently stirred emulsification, and initiator is added in mixing time 30min, and initiator selects hydrop isopropyl
Benzole soln makes to start polymerization reaction in mixed emulsion, and heat of polymerization is warming up to 90 degree after discharging, keep the temperature 2 hours, reacted
At；
(4) it agglomerates: after polymerization reaction 2 hours, material being arranged to collection surface, it is broken that polymerization inhibitor stirring 30min addition is added
Emulsion is demulsified to obtain target product under the conditions of 70~75 DEG C, carries out carrying out under 50~60 DEG C of water temperatures respectively later more
It is secondary to wash glue；
(5) drying glue, packaging: carrying out air-dried at 100~110 DEG C, then carries out cutting packaging to rubber.
2, experimental result
2.1 acrylonitrile and methyl acrylate accounting influence measurement result to intensity and compression set
In order to confirm that methyl acrylate and acrylonitrile accounting can be to acrylic rubber intensity and compression set shadow
It rings, is sampled after the completion of drying glue.Experiment condition is as follows: sample 1, sample 2, sample 3, sample 4, sample 5 be respectively embodiment 1,
Embodiment 2, embodiment 3, embodiment 4, the condition and dosage of embodiment 5.It is as shown in table 1 through experimental analysis data.
1 acrylonitrile of table and methyl acrylate accounting influence measurement result to intensity and compression set
Table 1
It can be obtained according to above-mentioned experimental result and table 1, in the case that other compositions are basically unchanged, change enhancing monomer third
The tensile strength of the accounting of alkene nitrile, the higher rubber of accounting is bigger, and when the concentration of acrylonitrile and methyl acrylate is constant, change is added
The amount of methyl acrylate, as the accounting of methyl acrylate is higher and higher, the permanent compression set of gained experimental product is lower, according to
According to the acrylic rubber that this method manufactures, by the way that enhancing monomer and carboxylic acid type cross-linking monomer are added in rubber, due to it
The presence of carboxyl thus has good permanent compression set, and at 150 DEG C, in the case of 48h, buckling changes from 20-28, and due to
The effect for enhancing monomer has the higher-strength for being greater than 15MPa.
2.2 methyl acrylate additive amounts influence acrylic rubber tensile strength
2 methyl acrylate additive amount of table influences acrylic rubber tensile strength
The present invention has studied methyl acrylate to acrylic rubber intensity effect, sample 6-10 other conditions with implementation
Example 1 is identical, and experimental result is as shown in table 2.By comparison as can be seen that methyl acrylate accounting improves, rubber tensile intensity is mentioned
It is high.
2.3 acrylonitrile additive amounts influence acrylic rubber tensile strength
3 acrylonitrile additive amount of table influences acrylic rubber tensile strength
Table 3
The present invention has studied acrylonitrile to acrylic rubber intensity effect, sample 11-15 other conditions with embodiment 1
Identical, experimental result is as shown in table 3.By comparison as can be seen that acrylonitrile accounting improves, rubber tensile intensity is improved.
2.4 acrylonitrile and methyl acrylate accounting are constant, and the two proportion variation is to intensity effect measurement result
According to table 1, acrylonitrile and when the total accounting 10% of methyl acrylate, tensile strength highest, in order to confirm propylene
Sour methyl esters and acrylonitrile account for entire material 10%, and matching variation between the two influences acrylic rubber, through experimental analysis
Data are as shown in table 4.
4 acrylonitrile of table and methyl acrylate accounting 10%, the two proportion variation is to intensity effect measurement result
| Sampling test parameter | Acrylonitrile: methyl acrylate | Tensile strength (MPA) | Elongation rate of tensile failure (%) |
| Sample 16 | 2:8 | 13.4 | ≥200 |
| Sample 17 | 5:5 | 18 | ≥200 |
| Sample 18 | 4:6 | 15.6 | ≥200 |
| Sample 19 | 8:2 | 15.1 | ≥200 |
Table 4
It can be obtained according to above-mentioned experimental result and table 4, in the case that other compositions are basically unchanged, methyl acrylate and third
Alkene nitrile entirety accounting is 10%, and change matches between the two, and acrylic rubber intensity increases, as accounting 5:5 between the two,
Rubber tensile intensity is best.
Above-mentioned technical proposal only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art
The principle of the present invention is embodied to some variations that some of them part may be made, belongs to the scope of protection of the present invention it
It is interior.
Claims (9)
1. a kind of method of high intensity carboxyl type acrylic rubber, which comprises the following steps: step S1, determination
Raw material ratio；Step S2, prepared by small powder；Step S3, raw material premix；Step S4, emulsion polymerization；Step S5, demulsification cohesion；Step
Rapid S6, glue is washed；Step S7, it dries；Step S8, it packs；
Step S1: main monomer chooses butyl acrylate and ethyl acrylate (the two accounting 70%-85%), methyl acrylate or
Acrylonitrile is as enhancing monomer (accounting 10%-15%), one of acrylic acid, maleic acid and itaconic acid or two kinds of conducts
Cross-linking monomer (10%-5%)；
Step S2: configuration small powder, small powder includes: molecular weight regulator, polymerization inhibitor and demulsifier；
Step S3: main monomer and cross-linking monomer are added in premix kettle and is configured to premix, the time about 30 minutes；
Step S4: being added water in a kettle, and emulsifier (lauryl sodium sulfate+OP-10) stirring of 1%-6% is then added
30 minutes, lotion is made.The premix raw material premixed in kettle is added in lotion again, emulsification, mixing time 30min is sufficiently stirred.It protects
Hold temperature 30 --- 90 degree, initiator (cumyl hydroperoxide) is added into lotion, reaction starts.
Step S5: after reacting 1~8 hour in step s 4, material being arranged to collection surface, and polymerization inhibitor stirring 30min is added and is added
Demulsifier is demulsified to obtain target product under the conditions of 70~75 DEG C；
Step S6: the obtained carboxyl type acrylic rubber in step S5 is subjected to abundant water under 45~82 DEG C of water temperature
It washes；
Step S7: the carboxyl type acrylic rubber after washing is dried in the environment of 70~120 DEG C of temperature；
Step S8: the carboxyl type acrylic rubber after drying is subjected to cutting packaging.
2. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
Methyl methacrylate accounting in rapid S1 is 5%~10%, acrylonitrile accounting is 5%~10%.
3. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
A length of half an hour when stirring in rapid S3.
4. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
After initiator is added in rapid S4, the thiol solution of concentration 1.05%~1.1% is selected to be added to polymerization as molecular weight regulator
In lotion.
5. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
Polymerization inhibitor selects hydroquinone in rapid S5, and its additive capacity is a ten thousandth as mass fraction.
6. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
It is 1% sodium chloride solution that the demulsifier added in rapid S5, which selects mass fraction,.
7. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 4, which is characterized in that the step
It is 70~80 DEG C that temperature of reaction kettle is kept in rapid S4 polymerization process, and the reaction time is 2 hours.
8. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
Water temperature in rapid S6 is set as 50~60 DEG C.
9. a kind of method of high-intensitive carboxyl type acrylic rubber according to claim 1, which is characterized in that the step
Drying temperature in rapid S7 is set as 100~110 DEG C.
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| CN (1) | CN110498881A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019040A (en) * | 2019-12-31 | 2020-04-17 | 山东海益橡胶科技有限公司 | High-strength non-stick roll acrylate rubber, preparation method thereof and vulcanized rubber composition composed of high-strength non-stick roll acrylate rubber |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2686772A (en) * | 1952-04-16 | 1954-08-17 | Rohm & Haas | N, n-ethyleneureido esters of acrylic and methacrylic acids |
| CN101993511A (en) * | 2009-08-28 | 2011-03-30 | 袁文阳 | Cold-resistant acrylate rubber as well as preparation and application thereof |
| CN102993354A (en) * | 2012-10-24 | 2013-03-27 | 宿迁市英杰装饰材料有限公司 | Frigostabile elastic acrylic ester copolymerization emulsion |
| CN105085786A (en) * | 2015-08-26 | 2015-11-25 | 常州海霸橡胶有限公司 | Preparation method of low-compression permanent-deformation carboxylic acrylate rubber |
| CN107325223A (en) * | 2017-07-17 | 2017-11-07 | 安徽华晶新材料有限公司 | A kind of environmental type preparation method of ACM |
| CN109265600A (en) * | 2018-09-10 | 2019-01-25 | 四川道弘新材料有限公司 | A kind of preparation method of double activated acrylic rubber |
-
2019
- 2019-07-16 CN CN201910639235.8A patent/CN110498881A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2686772A (en) * | 1952-04-16 | 1954-08-17 | Rohm & Haas | N, n-ethyleneureido esters of acrylic and methacrylic acids |
| CN101993511A (en) * | 2009-08-28 | 2011-03-30 | 袁文阳 | Cold-resistant acrylate rubber as well as preparation and application thereof |
| CN102993354A (en) * | 2012-10-24 | 2013-03-27 | 宿迁市英杰装饰材料有限公司 | Frigostabile elastic acrylic ester copolymerization emulsion |
| CN105085786A (en) * | 2015-08-26 | 2015-11-25 | 常州海霸橡胶有限公司 | Preparation method of low-compression permanent-deformation carboxylic acrylate rubber |
| CN107325223A (en) * | 2017-07-17 | 2017-11-07 | 安徽华晶新材料有限公司 | A kind of environmental type preparation method of ACM |
| CN109265600A (en) * | 2018-09-10 | 2019-01-25 | 四川道弘新材料有限公司 | A kind of preparation method of double activated acrylic rubber |
Non-Patent Citations (2)
| Title |
|---|
| 杨奇等: "一种具有优良特性橡胶的研究", 《陕西理工学院学报》 * |
| 杨奇等: "高强度高伸长率丙烯酸酯橡胶的合成研究", 《现代化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111019040A (en) * | 2019-12-31 | 2020-04-17 | 山东海益橡胶科技有限公司 | High-strength non-stick roll acrylate rubber, preparation method thereof and vulcanized rubber composition composed of high-strength non-stick roll acrylate rubber |
| CN111019040B (en) * | 2019-12-31 | 2021-01-08 | 山东海益橡胶科技有限公司 | High-strength non-stick roll acrylate rubber, preparation method thereof and vulcanized rubber composition composed of high-strength non-stick roll acrylate rubber |
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