CN103588928A - Preparation method for polyacrylate rubber - Google Patents
Preparation method for polyacrylate rubber Download PDFInfo
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- CN103588928A CN103588928A CN201310550355.3A CN201310550355A CN103588928A CN 103588928 A CN103588928 A CN 103588928A CN 201310550355 A CN201310550355 A CN 201310550355A CN 103588928 A CN103588928 A CN 103588928A
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Abstract
The invention belongs to the technical field of rubber production and in particular relates to a preparation method for polyacrylate rubber. The preparation method comprises the following steps: (1) preparing materials; (2) emulsifying; (3), polymerizing; (4) demulsifying to obtain the polyacrylate rubber. The method is simple to operate, low in production cost and high in yield of the polyacrylate rubber; the polyacrylate rubber prepared by the method is greatly improved in low temperature resistance and processing performance and is also improved in high temperature resistance.
Description
Technical field
The invention belongs to the technical field of rubber production, be specifically related to a kind of preparation method of polyacrylic rubber.
Background technology
Polyacrylic rubber is called for short ACM, is a kind of oil-proofness and stable on heating specialty elastomer, and owing to having very high cost performance, polyacrylic rubber is widely used in oil sealing field, such as automobile oil seal, transformer sealing etc.The macromolecular main chain of polyacrylic rubber is saturated, on its side chain with the very strong ester group of polarity, this structure makes polyacrylic rubber have outstanding thermotolerance, the swelling property of resistance to hydrocarbon-type oil, and resistance to low temperature is not ideal enough, processing difficulties, easy roll banding, these 2 application that seriously restrict polyacrylic rubber.
Along with Hyundai Motor is to high speed, energy saving direction development, make the requirement of automobile cylinder temperature of combustion improve constantly,
Cause the SC service ceiling temperature requirement of sealing material used to be also enhanced.Require in the past acrylic elastomer sealing member at 150 ℃
Time life-time service, brought up to gradually now 170 ℃ of even higher temperatures, ACM prepared by conventional emulsion polymerization technique can not meet the demands.How current ACM obtains ideal bound and the long lifetime of high thermal resistance, also has low cost and good productivity technique concurrently simultaneously, has become the problem that this field must be faced.
Summary of the invention
The object of the invention is to for the defect of above-mentioned existence and a kind of preparation method of polyacrylic rubber is provided, the method is simple to operate, reduces production costs, and has improved the yield of polyacrylic rubber; Use the prepared polyacrylic rubber of the method, greatly strengthened resistance to low temperature and processing characteristics; Also improved the resistance to elevated temperatures of polyacrylic rubber simultaneously.
Technical scheme of the present invention is: a kind of preparation method of polyacrylic rubber, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is (15~35): 1, and the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is (10~20): 1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is (2~3): 1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is (3~5): 1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 30~35 ℃, and emulsification times is 45~50 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 45~50 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 60~80 ℃, reacts 2~5 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 5~7% sodium chloride solution, carries out breakdown of emulsion under 70~75 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
Described polyacrylic rubber preparation method, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 30:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 15:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 2.5:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 4.5:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 32 ℃, and emulsification times is 47 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 48 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 75 ℃, reacts 4 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 6% sodium chloride solution, carries out breakdown of emulsion under 72 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
In described step (3), the weight percent of initiator and raw emulsion is (0.01~1.5): 1.
In described step (3), the weight percent of initiator and raw emulsion is 0.06:1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is (0.5~1): 1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 0.8:1.
Beneficial effect of the present invention is: the preparation method of polyacrylic rubber of the present invention has improved the yield of polyacrylic rubber greatly, makes its yield reach 75~88%; Adopt this preparation method to make the polyacrylic rubber maximum operation (service) temperature obtaining reach 220~280 ℃; And constant product quality is high.The method is simple to operate, reduces production costs, and has improved the yield of polyacrylic rubber; Use the prepared polyacrylic rubber of the method, greatly strengthened resistance to low temperature and processing characteristics; Also improved the resistance to elevated temperatures of polyacrylic rubber simultaneously.
Embodiment
Below by specific embodiment, the present invention will be described in detail.
Embodiment 1
A preparation method for polyacrylic rubber, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 15:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 10:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 2:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 3:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 30 ℃, and emulsification times is 45 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 45 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 60 ℃, reacts 2 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 5% sodium chloride solution, carries out breakdown of emulsion under 70 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
In described step (3), the weight percent of initiator and raw emulsion is 0.01:1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 0.5:1.
Adopting the yield of the present embodiment 1 polyacrylic rubber is 77%, and polyacrylic rubber maximum operation (service) temperature reaches 220 ℃
Embodiment 2
Described polyacrylic rubber preparation method, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 30:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 15:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 2.5:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 4.5:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 32 ℃, and emulsification times is 47 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 48 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 75 ℃, reacts 4 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 6% sodium chloride solution, carries out breakdown of emulsion under 72 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
In described step (3), the weight percent of initiator and raw emulsion is 0.06:1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 0.8:1.
Adopting the yield of the present embodiment 2 polyacrylic rubbers is 88%, and polyacrylic rubber maximum operation (service) temperature reaches 280 ℃
Embodiment 3
A preparation method for polyacrylic rubber, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 35:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 20:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 3:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 5:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 35 ℃, and emulsification times is 50 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 50 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 80 ℃, reacts 5 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 7% sodium chloride solution, carries out breakdown of emulsion under 75 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
In described step (3), the weight percent of initiator and raw emulsion is 1.5:1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 1:1.
Adopting the yield of the present embodiment 1 polyacrylic rubber is 80%, and polyacrylic rubber maximum operation (service) temperature reaches 250 ℃
Embodiment 4
A preparation method for polyacrylic rubber, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 20:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 12:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 2.3:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 3.5:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 33 ℃, and emulsification times is 46 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 48 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 77 ℃, reacts 4 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 6% sodium chloride solution, carries out breakdown of emulsion under 74 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
In described step (3), the weight percent of initiator and raw emulsion is 1.2:1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 0.8:1.
Adopting the yield of the present embodiment 1 polyacrylic rubber is 78%, and polyacrylic rubber maximum operation (service) temperature reaches 270 ℃
Embodiment 5
A preparation method for polyacrylic rubber, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 33:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 19:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 2.3:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 4.6:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 32 ℃, and emulsification times is 46
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 48 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 76 ℃, reacts 3.5 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 7% sodium chloride solution, carries out breakdown of emulsion under 72 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
In described step (3), the weight percent of initiator and raw emulsion is 1.4:1.
In described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 0.6:1.
Adopting the yield of the present embodiment 1 polyacrylic rubber is 80%, and polyacrylic rubber maximum operation (service) temperature reaches 250 ℃.
Claims (6)
1. a preparation method for polyacrylic rubber, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is (15~35): 1, and the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is (10~20): 1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is (2~3): 1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is (3~5): 1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 30~35 ℃, and emulsification times is 45~50 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 45~50 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 60~80 ℃, reacts 2~5 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 5~7% sodium chloride solution, carries out breakdown of emulsion under 70~75 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
2. polyacrylic rubber preparation method according to claim 1, comprises the following steps:
(1) preparation: raw material is formulated by butyl acrylate, methyl-propyl acid methyl esters and ethyl acetate, wherein the weight ratio of butyl acrylate and methyl-propyl acid methyl esters is 30:1, the weight ratio of ethyl acetate and methyl-propyl acid methyl esters is 15:1; Emulsifying agent is formulated by dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium, and wherein the weight ratio of dodecyl oxygen acid sodium and alkyl oxy DAADBSA disodium is 2.5:1; Initiator is formulated by Diisopropyl azodicarboxylate and ammonium persulphate, and wherein the weight ratio of Diisopropyl azodicarboxylate and ammonium persulphate is 4.5:1;
(2) emulsification: emulsifying agent is added in raw material, raw material is carried out to emulsification, emulsifying temperature is 32 ℃, and emulsification times is 47 minutes, obtains raw emulsion;
(3) polymerization: will add initiator in the resulting raw emulsion of step (2), initiated polymerization under 48 ℃ of conditions, then maintains temperature of reaction and carry out polyreaction at 75 ℃, reacts 4 hours, obtains polyacrylate dispersion;
(4) breakdown of emulsion: adding mass percent in the polyacrylate dispersion of step (3) gained is 6% sodium chloride solution, carries out breakdown of emulsion under 72 ℃ of conditions, gained solid, after washing, dehydration, drying, makes polyacrylic rubber.
3. polyacrylic rubber preparation method according to claim 1 and 2, is characterized in that, in described step (3), the weight percent of initiator and raw emulsion is (0.01~1.5): 1.
4. polyacrylic rubber preparation method according to claim 3, is characterized in that, in described step (3), the weight percent of initiator and raw emulsion is 0.06:1.
5. polyacrylic rubber preparation method according to claim 1 and 2, is characterized in that, in described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is (0.5~1): 1.
6. polyacrylic rubber preparation method according to claim 5, is characterized in that, in described step (4), the weight ratio of sodium chloride solution and polyacrylate dispersion is 0.8:1.
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Cited By (3)
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CN110498880A (en) * | 2019-07-16 | 2019-11-26 | 九江杜威橡胶科技有限公司 | A kind of manufacturing method of extremely cold-resistant carboxyl type acrylic rubber |
CN110498882A (en) * | 2019-07-16 | 2019-11-26 | 九江杜威橡胶科技有限公司 | A kind of butadiene is the preparation method of the universal acrylic rubber of polymerized monomer |
CN110527013A (en) * | 2019-07-16 | 2019-12-03 | 九江杜威橡胶科技有限公司 | A kind of preparation method of the double cross-linked acrylate rubbers of hardy type |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110498880A (en) * | 2019-07-16 | 2019-11-26 | 九江杜威橡胶科技有限公司 | A kind of manufacturing method of extremely cold-resistant carboxyl type acrylic rubber |
CN110498882A (en) * | 2019-07-16 | 2019-11-26 | 九江杜威橡胶科技有限公司 | A kind of butadiene is the preparation method of the universal acrylic rubber of polymerized monomer |
CN110527013A (en) * | 2019-07-16 | 2019-12-03 | 九江杜威橡胶科技有限公司 | A kind of preparation method of the double cross-linked acrylate rubbers of hardy type |
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