CN104262528A - Preparation method for flame-retardant acrylic rubber - Google Patents
Preparation method for flame-retardant acrylic rubber Download PDFInfo
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- CN104262528A CN104262528A CN201410532118.9A CN201410532118A CN104262528A CN 104262528 A CN104262528 A CN 104262528A CN 201410532118 A CN201410532118 A CN 201410532118A CN 104262528 A CN104262528 A CN 104262528A
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Abstract
The invention relates to a preparation method for flame-retardant acrylic rubber. According to the preparation method, the problem that the flame-retardant performance of the acrylic rubber in the prior art is poorer is mainly solved. The preparation method for the flame-retardant acrylic rubber, disclosed by the invention, comprises the following steps: under an inert gas atmosphere, adding a main acrylate monomer, a flame-retardant monomer, a cross-linking monomer and a chain transfer agent in a water system containing an emulsifying agent; emulsifying the mixture at the temperature of 40-90DEG C; then adding an initiator for reacting; finally, coagulating, washing and drying the emulsion obtained by reacting to obtain the flame-retardant acrylic rubber, wherein the flame-retardant monomer is a monomer containing double bonds and a phosphate ester group; according to the technical scheme adopted by the invention, the problems are better solved; the preparation method can be used for preparing the flame-retardant acrylic rubber.
Description
Technical field
The present invention relates to a kind of preparation method of Flame-retardant acrylic acid ester rubber.
Background technology
Acrylic elastomer (hereinafter referred to as ACM) take acrylate as the elastomerics that main monomer obtains through copolymerization, its main chain is saturated carbon chains, side base is polar ester groups, the feature of its many excellence given by special construction, as high-low temperature resistant, ageing-resistant, oil resistant, resistance to ozone, uvioresistant etc.CN03117291.1 relates to a kind of preparation method with the acrylic elastomer of two/many components cure site monomer, with acrylate monomer with there is the monomer of crosslinking activity group for raw material on a small quantity, adopt emulsion polymerization.Generate multipolymer, it is characterized in that, aforesaid propylene acid ester monomer raw material be one of following kinds or several: ethyl propenoate, butyl acrylate, methoxyethyl acrylate, ethoxyethyl acrylate; The above-mentioned monomer with crosslinking activity group is select two or more in following kinds: vinyl monochloroacetate, vinyl cyanide, vinylformic acid, glycidyl ether, glycidyl acrylate, ethylidene norbornene.It has vulcanization characteristics widely, and arbitrary or whole curable monomer component in sizing material can be utilized to carry out cross-linking vulcanized reaction, solves existing kind to the comparatively narrow problem of vulcanizing agent range of choice.
Although ACM has been widely used in all kinds of oil-resistant high-temperature sealing members of automobile etc., Application Areas has still had limitation.Cable sheath and resin toughening modification be its application extended field, and its low cigarette and flame-retarding power still not enough, its flame retardant resistance is urgently to be resolved hurrily.Usually two kinds of method of modifying are had: physically modified and chemical modification.Relative physically modified, chemical modification tool has the following advantages: (1) improves the consistency of polymkeric substance and flame-retardant monomer.(2) little to the Effect on Mechanical Properties of polymkeric substance.(3) service efficiency is high, just can improve fire resistance with a small amount of flame-retardant monomer.Therefore chemically modification angle is set out, research and development Flame-retardant acrylic acid ester rubber important in inhibiting.
Summary of the invention
Technical problem to be solved by this invention is the problem that in prior art, the flame retardant properties of acrylic elastomer is poor, provides a kind of preparation method of new Flame-retardant acrylic acid ester rubber.The method is used for, in the preparation of Flame-retardant acrylic acid ester rubber, having the good advantage of flame retardant properties of acrylic elastomer.
For solving the problem, the technical solution used in the present invention is as follows: a kind of preparation method of Flame-retardant acrylic acid ester rubber, under inert gas atmosphere, to containing in the aqueous systems of emulsifying agent, add acrylate main monomer, flame-retardant monomer, cross-linking monomer, chain-transfer agent, emulsified at 40 ~ 90 DEG C, then add initiator and react, finally the emulsion be obtained by reacting is carried out condensing, washing and drying, obtain Flame-retardant acrylic acid ester rubber; Wherein, described flame-retardant monomer is the monomer containing double bond and bound phosphate groups.
In technique scheme, preferably, water is deionized water, and described rare gas element is nitrogen.
In technique scheme, preferably, described acrylate main monomer is selected from least one in methyl acrylate, ethyl propenoate, butyl acrylate, 2-EHA, methoxyethyl acrylate, ethoxyethyl acrylate, methoxyethyl butyl ester; Described flame-retardant monomer is selected from least one in 2-ethyl (methacryloxymethyl) phosphonic acid ester, 2-ethyl (acryloyloxymethyl) phosphonic acid ester, 2-ethyl (methacryloxymethyl) phosphoric acid ester, methacrylic acid dibutoxy etherophosphoric acid; Described cross-linking monomer is selected from least one in carboxylic acid compound, epoxy compounds, halide-containing, diolefin; Chain-transfer agent is selected from least one in Dodecyl Mercaptan or tert-dodecyl mercaptan; Described emulsifying agent is selected from least one in nonionic emulsifier, lipid acid, anionic emulsifier; Initiator is selected from least one in azo-compound, organo-peroxide or inorganic peroxide.
In technique scheme, more preferably, carboxylic acid compound is selected from vinylformic acid, fumaric acid; Epoxy compounds is selected from glycidyl methacrylate; Halide-containing is selected from chloracetic acid vinyl acetate; Diolefin is selected from ethylidene norbornene; Nonionic emulsifier is selected from Voranol EP 2001, polyxyethylated alkylphenol, polyxyethylated ester; Emulsifying agent is selected from anionic emulsifier, and anionic emulsifier is selected from sodium laurylsulfonate, sodium lauryl sulphate; Lipid acid is selected from oleic acid, linolenic acid; Azo-compound is selected from Diisopropyl azodicarboxylate; Organo-peroxide is selected from di-isopropylbenzene hydroperoxide, hydrogen phosphide cumene, benzoyl peroxide; Inorganic peroxide is selected from Potassium Persulphate, ammonium persulphate.
In technique scheme, preferably, the consumption mass ratio of described flame-retardant monomer and acrylate main monomer is 1:90 ~ 5:85; The consumption mass ratio of cross-linking monomer and acrylate main monomer is 1:90 ~ 5:85; Relative to monomer mixture 100 weight part, emulsifier is 0.1 ~ 10 weight part, and initiator amount is 0.01 ~ 1.0 weight part, and chain-transfer agent consumption is 0.0001 ~ 0.001 weight part, and the consumption of deionized water is 100 ~ 500 weight parts.
In technique scheme, more preferably, the consumption mass ratio of described flame-retardant monomer and acrylate main monomer is 2:89 ~ 3:88; The consumption mass ratio of cross-linking monomer and acrylate main monomer is 2:89 ~ 3:88; Relative to monomer mixture 100 weight part, emulsifier is 2 ~ 5 weight parts, and initiator amount is 0.2 ~ 0.5 weight part, and chain-transfer agent consumption is 0.0004 ~ 0.0007 weight part, and the consumption of deionized water is 200 ~ 300 weight parts.
In technique scheme, preferably, after 40 ~ 90 DEG C of emulsified 0.3 ~ 2h, add initiator, react 1 ~ 6 hour.
In technique scheme, more preferably, after 60 ~ 70 DEG C of emulsified 0.5 ~ 1h, add initiator, react 3 ~ 5 hours.
The present invention carries out copolymerization by phosphoric acrylic ester monomer and conventional acrylates monomer, introduces organic phosphate flame-retardant group, gives acrylic elastomer flame retardant resistance, the mooney viscosity (ML100 DEG C of the Flame-retardant acrylic acid ester rubber utilizing the present invention to prepare
1+4) be 30 ~ 50, limiting oxygen index(LOI) (LOI) is 24 ~ 28, has good flame retardant effect.Method of the present invention not only increases the flame retardant properties of acrylic elastomer, and less to the Effect on Mechanical Properties of rubber, achieves good technique effect.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
In a nitrogen atmosphere, add 64g deionized water in there-necked flask, 0.64g sodium laurylsulfonate, hierarchy of control temperature at 50 DEG C, and constantly stirs.Weigh ethyl propenoate 32g subsequently, 2-ethyl (methacryloxymethyl) phosphonic acid ester 0.72g, glycidyl methacrylate 0.72g, Diisopropyl azodicarboxylate 0.064g is added after emulsification 0.5h, after reaction 4h, then the emulsion be obtained by reacting is carried out condense, to wash and namely drying prepares Flame-retardant acrylic acid ester rubber.Mooney viscosity (ML100 DEG C
1+4) be 35, limiting oxygen index(LOI) (LOI) is 25.
[embodiment 2]
In a nitrogen atmosphere, add 70g deionized water in there-necked flask, 0.32g sodium lauryl sulphate, hierarchy of control temperature at 70 DEG C, and constantly stirs.Weigh butyl acrylate 32g subsequently, methacrylic acid dibutoxy etherophosphoric acid 0.6g, vinylformic acid 0.6g, Dodecyl Mercaptan 0.016g, Potassium Persulphate 0.032g is added after emulsification 1h, after reaction 6h, then the emulsion be obtained by reacting is carried out condense, to wash and namely drying prepares Flame-retardant acrylic acid ester rubber.Mooney viscosity (ML100 DEG C
1+4) be 41, limiting oxygen index(LOI) (LOI) is 26.
[embodiment 3]
In a nitrogen atmosphere, add 96g deionized water in there-necked flask, 0.32g polyxyethylated alkylphenol, hierarchy of control temperature at 60 DEG C, and constantly stirs.Weigh ethyl propenoate 16g subsequently, butyl acrylate 16g, 2-ethyl (methacryloxymethyl) phosphoesterase 30 .56g, chloracetic acid vinyl acetate 0.56g, Dodecyl Mercaptan 0.008g, add di-isopropylbenzene hydroperoxide 0.016g after emulsification 1h, after reaction 3h, then the emulsion be obtained by reacting is carried out condense, to wash and namely drying prepares Flame-retardant acrylic acid ester rubber.Mooney viscosity (ML100 DEG C
1+4) be 37, limiting oxygen index(LOI) (LOI) is 28.
[embodiment 4]
In a nitrogen atmosphere, add 96g deionized water in there-necked flask, 0.16g sodium laurylsulfonate, the polyxyethylated ester of 0.16g, hierarchy of control temperature at 70 DEG C, and constantly stirs.Weigh ethyl propenoate 16g subsequently, ethoxyethyl acrylate 16g, 2-ethyl (acryloyloxymethyl) phosphonic acid ester 0.6g, ethylidene norbornene 0.12g, tert-dodecyl mercaptan 0.016g, adds benzoyl peroxide 0.012g after emulsification 1h, after reaction 5h, the emulsion be obtained by reacting is carried out condense, wash and drying, prepare Flame-retardant acrylic acid ester rubber.Mooney viscosity (ML100 DEG C
1+4) be 47, limiting oxygen index(LOI) (LOI) is 25.
[embodiment 5]
In a nitrogen atmosphere, add 64g deionized water in there-necked flask, 0.16g sodium lauryl sulphate, the polyxyethylated ester of 0.16g, hierarchy of control temperature at 65 DEG C, and constantly stirs.Weigh ethyl propenoate 16g subsequently, butyl acrylate 8g, ethoxyethyl acrylate 8g, 2-ethyl (acryloyloxymethyl) phosphonic acid ester 0.5g, methacrylic acid dibutoxy etherophosphoric acid 0.5g, chloracetic acid vinyl acetate 0.06g, ethylidene norbornene 0.06g, tert-dodecyl mercaptan 0.02g, ammonium persulphate 0.032g is added after emulsification 1h, after reaction 4h, the emulsion be obtained by reacting is carried out condense, wash and drying, prepare Flame-retardant acrylic acid ester rubber.Mooney viscosity (ML100 DEG C
1+4) be 37, limiting oxygen index(LOI) (LOI) is 24.
[embodiment 6]
In a nitrogen atmosphere, add 70g deionized water in there-necked flask, 0.16g sodium lauryl sulphate, the polyxyethylated ester of 0.16g, hierarchy of control temperature at 60 DEG C, and constantly stirs.Weigh ethyl propenoate 12g subsequently, butyl acrylate 12g, methyl methacrylate 12g, 2-ethyl (methacryloxymethyl) phosphonic acid ester 0.8g, methacrylic acid dibutoxy phosphoric acid 0.8g, chloracetic acid vinyl acetate 0.6g, methyl propenoic acid glycidyl ether 0.6g, ethylidene norbornene 0.6g, tert-dodecyl mercaptan 0.02g, adds ammonium persulphate 0.1g after emulsification 1h, after reaction 6h, the emulsion be obtained by reacting is carried out condense, wash and drying, prepare Flame-retardant acrylic acid ester rubber.Mooney viscosity (ML100 DEG C
1+4) be 40, limiting oxygen index(LOI) (LOI) is 28.
Claims (8)
1. the preparation method of a Flame-retardant acrylic acid ester rubber, under inert gas atmosphere, to containing in the aqueous systems of emulsifying agent, add acrylate main monomer, flame-retardant monomer, cross-linking monomer, chain-transfer agent, emulsified at 40 ~ 90 DEG C, then add initiator to react, finally the emulsion be obtained by reacting is carried out condensing, washing and drying, obtain Flame-retardant acrylic acid ester rubber; Wherein, described flame-retardant monomer is the monomer containing double bond and bound phosphate groups.
2. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 1, it is characterized in that described water is deionized water, rare gas element is nitrogen.
3. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 1, is characterized in that described acrylate main monomer is selected from least one in methyl acrylate, ethyl propenoate, butyl acrylate, 2-EHA, methoxyethyl acrylate, ethoxyethyl acrylate, methoxyethyl butyl ester; Described flame-retardant monomer is selected from least one in 2-ethyl (methacryloxymethyl) phosphonic acid ester, 2-ethyl (acryloyloxymethyl) phosphonic acid ester, 2-ethyl (methacryloxymethyl) phosphoric acid ester, methacrylic acid dibutoxy etherophosphoric acid; Described cross-linking monomer is selected from least one in carboxylic acid compound, epoxy compounds, halide-containing, diolefin; Chain-transfer agent is selected from least one in Dodecyl Mercaptan or tert-dodecyl mercaptan; Described emulsifying agent is selected from least one in nonionic emulsifier, lipid acid, anionic emulsifier; Initiator is selected from least one in azo-compound, organo-peroxide or inorganic peroxide.
4. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 3, is characterized in that carboxylic acid compound is selected from vinylformic acid, fumaric acid; Epoxy compounds is selected from glycidyl methacrylate; Halide-containing is selected from chloracetic acid vinyl acetate; Diolefin is selected from ethylidene norbornene; Nonionic emulsifier is selected from Voranol EP 2001, polyxyethylated alkylphenol, polyxyethylated ester; Emulsifying agent is selected from anionic emulsifier, and anionic emulsifier is selected from sodium laurylsulfonate, sodium lauryl sulphate; Lipid acid is selected from oleic acid, linolenic acid; Azo-compound is selected from Diisopropyl azodicarboxylate; Organo-peroxide is selected from di-isopropylbenzene hydroperoxide, hydrogen phosphide cumene, benzoyl peroxide; Inorganic peroxide is selected from Potassium Persulphate, ammonium persulphate.
5. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 1, is characterized in that the consumption mass ratio of described flame-retardant monomer and acrylate main monomer is 1:90 ~ 5:85; The consumption mass ratio of cross-linking monomer and acrylate main monomer is 1:90 ~ 5:85; Relative to monomer mixture (mixture of acrylate main monomer, flame-retardant monomer, cross-linking monomer) 100 weight parts, emulsifier is 0.1 ~ 10 weight part, initiator amount is 0.01 ~ 1.0 weight part, chain-transfer agent consumption is 0.0001 ~ 0.001 weight part, and the consumption of deionized water is 100 ~ 500 weight parts.
6. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 5, is characterized in that the consumption mass ratio of described flame-retardant monomer and acrylate main monomer is 2:89 ~ 3:88; The consumption mass ratio of cross-linking monomer and acrylate main monomer is 2:89 ~ 3:88; Relative to monomer mixture 100 weight part, emulsifier is 2 ~ 5 weight parts, and initiator amount is 0.2 ~ 0.5 weight part, and chain-transfer agent consumption is 0.0004 ~ 0.0007 weight part, and the consumption of deionized water is 200 ~ 300 weight parts.
7. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 1, is characterized in that adding initiator after 40 ~ 90 DEG C of emulsified 0.3 ~ 2h, reacts 1 ~ 6 hour.
8. the preparation method of Flame-retardant acrylic acid ester rubber according to claim 7, is characterized in that adding initiator after 60 ~ 70 DEG C of emulsified 0.5 ~ 1h, reacts 3 ~ 5 hours.
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Cited By (9)
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| CN106478880A (en) * | 2016-10-16 | 2017-03-08 | 韶关市连邦环保新材料股份有限公司 | A kind of polyacrylate resin and preparation method thereof |
| CN106554461A (en) * | 2016-12-01 | 2017-04-05 | 重庆金茂达特种橡胶有限公司 | The method for preparing high Mooney viscosity polyacrylate composition |
| CN107434838A (en) * | 2016-05-27 | 2017-12-05 | 台光电子材料股份有限公司 | Phosphorus-containing olefin polymer, preparation method thereof, composition thereof and finished product |
| CN108641257A (en) * | 2016-07-22 | 2018-10-12 | 吴振彪 | A kind of high temperature resistant acrylic rubber |
| CN109251268A (en) * | 2018-09-10 | 2019-01-22 | 四川道弘新材料有限公司 | A kind of preparation method of micro- cross-linked acrylate rubber |
| 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 |
| CN110157133A (en) * | 2019-06-17 | 2019-08-23 | 华北理工大学 | A kind of phosphoric acrylic ester elastomer fire retardant and preparation method thereof |
| CN111072846A (en) * | 2019-12-31 | 2020-04-28 | 山东海益橡胶科技有限公司 | Acrylate rubber capable of being directly vulcanized without washing and preparation method thereof |
| CN116034116A (en) * | 2020-06-05 | 2023-04-28 | 日本瑞翁株式会社 | Acrylic rubber excellent in roll processability, strength characteristics and water resistance |
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| CN107434838A (en) * | 2016-05-27 | 2017-12-05 | 台光电子材料股份有限公司 | Phosphorus-containing olefin polymer, preparation method thereof, composition thereof and finished product |
| CN108641257A (en) * | 2016-07-22 | 2018-10-12 | 吴振彪 | A kind of high temperature resistant acrylic rubber |
| CN106478880A (en) * | 2016-10-16 | 2017-03-08 | 韶关市连邦环保新材料股份有限公司 | A kind of polyacrylate resin and preparation method thereof |
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| CN106554461A (en) * | 2016-12-01 | 2017-04-05 | 重庆金茂达特种橡胶有限公司 | The method for preparing high Mooney viscosity polyacrylate composition |
| CN109251268A (en) * | 2018-09-10 | 2019-01-22 | 四川道弘新材料有限公司 | A kind of preparation method of micro- cross-linked acrylate rubber |
| 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 |
| CN110157133A (en) * | 2019-06-17 | 2019-08-23 | 华北理工大学 | A kind of phosphoric acrylic ester elastomer fire retardant and preparation method thereof |
| CN111072846A (en) * | 2019-12-31 | 2020-04-28 | 山东海益橡胶科技有限公司 | Acrylate rubber capable of being directly vulcanized without washing and preparation method thereof |
| CN116034116A (en) * | 2020-06-05 | 2023-04-28 | 日本瑞翁株式会社 | Acrylic rubber excellent in roll processability, strength characteristics and water resistance |
| CN116034116B (en) * | 2020-06-05 | 2024-03-26 | 日本瑞翁株式会社 | Acrylic rubber excellent in roll processability, strength characteristics and water resistance |
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