CN1100800C - Synthesis method for large grain size latex - Google Patents
Synthesis method for large grain size latex Download PDFInfo
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- CN1100800C CN1100800C CN00101339A CN00101339A CN1100800C CN 1100800 C CN1100800 C CN 1100800C CN 00101339 A CN00101339 A CN 00101339A CN 00101339 A CN00101339 A CN 00101339A CN 1100800 C CN1100800 C CN 1100800C
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Abstract
The present invention relates to a synthesis method of acrylic latex with large grain diameter. The method comprises the steps: 1) adding an emulsifying agent accounting for 0.01 to 0.09 wt% of the total amount of reaction monomers in a polymerization kettle; 2) adding monomers accounting for 30 to 60 wt% of the total amount of the reaction monomers in the polymerization kettle; 3) adding an initiating agent accounting for 0.2 to 0.8 wt% of the total amount of the reaction monomers into the polymerization kettle; 4) adding water in the polymerization kettle; completing charging; adding an emulsifying agent accounting for 0.2 to 0.8 wt% of the total amount of the reaction monomers and 40 to 70 wt% of residual monomers after temperature reaction for 15 to 20 minutes, wherein the emulsifying agent and the monomers can be added by one time or more times. After materials are loaded, the materials react for three to five hours in constant temperature; the grain diameter of the obtained latex is from 200 to 600 nm; the polymerization is completed in the same reaction kettle. The present invention has the advantages of short reaction time and low cost.
Description
The present invention relates to the synthetic method of latex, be specifically related to the emulsion polymerisation process of big particle diameter esters of acrylic acid latex.
The preparation large grain size latex is technological difficulties in the letex polymerization, mainly contains three kinds of method: A. at present and add inorganic electrolyte in polymerization system; B. reduce the emulsifying agent consumption; C. two-stage polymerization method.More than in three kinds of methods two kinds of methods of A, B all exist and amplify the shortcoming that grain size is limited, latex stability is relatively poor.In the letex polymerization of acrylic ester monomer, widely used is the two-stage polymerization method, be that the first step is earlier by the emulsion polymerization prepared seed latex, second step is on the basis of small particle size seed latex, add a certain amount of monomer once more and carry out letex polymerization, amplify particle diameter, adopt this method in 10 hours, can obtain the large grain size latex that median size is 410nm.Current two-stage polymerization method is to obtain the effective means of large grain size latex, but needs the two-stage polymerization process, long reaction time, and step is many.
The object of the present invention is to provide a kind of fast emulsion polymerisation process of synthetic big particle diameter esters of acrylic acid latex, be aggregated in the same reactor finish, the reaction times is shorter.
Synthetic main employing of esters of acrylic acid latex of the present invention adds the method for emulsion polymerization systems with reaction monomers and emulsifying agent gradation, thereby obtains the large grain size latex of 200-600nm at short notice.Concrete grammar is as follows: 1) add the emulsifying agent that accounts for reaction monomers total amount 0.01-0.09wt% to polymeric kettle; 2) add the reaction monomers that accounts for reaction monomers total amount 30-60wt% to polymeric kettle; 3) add the initiator that accounts for reaction monomers total amount 0.2-0.8wt% to polymeric kettle; 4) add entry to polymeric kettle; Reinforced finishing, add the emulsifying agent that accounts for the monomer of reaction monomers total amount 40-70wt% and account for reaction monomers total amount 0.2-0.8wt% after temperature reaction 15-20 minute again, this partial monosomy and emulsifying agent can be once or gradation add emulsion polymerization systems, reinforced finishing, isothermal reaction 3-5 hour, can make the big particle diameter esters of acrylic acid latex of 200-600nm.The monomer of suitable letex polymerization of the present invention comprises acrylic ester monomer, as methyl acrylate, methyl methacrylate, ethyl propenoate, Jia Jibingxisuanyizhi, butyl acrylate, butyl methacrylate, 2 ethyl hexyl acrylate, Octyl acrylate, Isooctyl acrylate monomer etc., and can with acrylic ester monomer crosslinking copolymerization polymeric monomer, as Vinylstyrene, ethylene glycol diacrylate, dimethacrylate second diester, diallyl phthalate etc.The emulsifying agent of suitable letex polymerization of the present invention comprises an alkali metal salt, sodium lauryl sulphate of an alkali metal salt, the Witco 1298 Soft Acid of senior lipid acid such as rosined soap, oleic acid, stearic acid etc., they can use separately also can mix use, wherein is preferably sodium lauryl sulphate.The initiator of suitable letex polymerization of the present invention is persulphate such as Potassium Persulphate, Sodium Persulfate, ammonium persulphate etc., can be used alone or as a mixture.
Gradation adds different emulsifying agent and the amount of monomer of measuring in letex polymerization by adopting in the present invention, thereby obtained the big particle diameter esters of acrylic acid latex of 200-600nm at 3～5 hours, had polymerization in same reactor, short, amplification effect outstanding feature of reaction times.
Embodiment one prescription: unit (g) butyl acrylate 300 ammonium persulphates 1.2 Sodium dodecylbenzene sulfonatees 3 water 360
At first in reactor, add emulsifying agent dodecyl benzene sulfonic acid sodium salt 0.03g and 100g butyl acrylate, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 15 minutes, add 200g butyl acrylate and 2.97g Sodium dodecylbenzene sulfonate, isothermal reaction 4 hours obtains latex particle size 390nm.
Embodiment two prescriptions: unit (g) butyl acrylate 200 ethyl propenoates 100 ammonium persulphates 1.2 Sodium dodecylbenzene sulfonatees 3 water 360
At first in reactor, add emulsifying agent dodecyl benzene sulfonic acid sodium salt 0.03g and 100g mix monomer, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 15-20 minute, add 200g mix monomer and 2.97g Sodium dodecylbenzene sulfonate, isothermal reaction 4 hours obtains latex particle size 380nm.
Embodiment three prescriptions: unit (g) methyl methacrylate 47 butyl acrylates 250 Vinylstyrenes 3 Potassium Persulphates 0.9 sodium lauryl sulphate 2.4 water 360
At first in reactor, add emulsifying agent dodecyl sodium sulfate 0.02g and 150g mix monomer, water 360g, initiator 0.9g, be warming up to 70 ℃ of reactions, react after 18 minutes, add 150g mix monomer and 2.38g sodium lauryl sulphate, isothermal reaction 4 hours obtains latex particle size 440nm.
Embodiment four prescriptions: unit (g) methyl methacrylate 50 ethyl propenoates 200 Octyl acrylates 50 Potassium Persulphates 0.6 sodium lauryl sulphate 2.0 Sodium dodecylbenzene sulfonatees 0.5 water 360
At first in reactor, add compound emulsifying agent 0.03g and 100g mix monomer, water 360g, initiator 0.6g, be warming up to 70 ℃ of reactions, react after 20 minutes, add 200g mix monomer and 2.47g compound emulsifying agent, isothermal reaction 3 hours obtains latex particle size 360nm.
Embodiment five prescriptions: unit (g) ethyl propenoate 290 dimethacrylate second diester 2 Potassium Persulphates 1.2 sodium lauryl sulphate 2 oleic acid 0.4 water 360
At first in reactor, add compound emulsifying agent 0.03g and 100g mix monomer, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 15 minutes, add 200g mix monomer and 2.37g compound emulsifying agent, isothermal reaction 4 hours obtains latex particle size 380nm.
Embodiment six: prescription: unit (g) methyl methacrylate 50 ethyl acrylates 200 EMAs 50 ammonium persulfates 1.2 lauryl sodium sulfate 2 rosin soaps 0.4 water 360
At first in reactor, add compound emulsifying agent 0.035g and 100g mix monomer, water 360g, initiator 1.2g is warming up to 70 ℃ of reactions, reacts after 16 minutes, add 100g mix monomer and 1.05g compound emulsifying agent, react after 30 minutes, add the 100g mix monomer again, the 1g compound emulsifying agent, isothermal reaction 5 hours obtains latex particle size 390nm.
Embodiment seven prescriptions: unit (g) butyl acrylate 296 Phthalic acid, diallyl esters 4 Potassium Persulphates 1.2 sodium lauryl sulphate 2.4 water 360
At first in reactor, add emulsifying agent dodecyl sodium sulfate 0.03g and 120g mix monomer, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 15 minutes, add 120g mix monomer and 1.37g sodium lauryl sulphate, react and add 60g mix monomer and 1g emulsifying agent after 30 minutes again, isothermal reaction 4 hours obtains latex particle size 398nm.
Embodiment eight: prescription: unit (g) Phthalic acid, diallyl ester 370 butyl acrylates 5 Potassium Persulphates 1.2 sodium lauryl sulphate 3.8 water 360
At first in reactor, add emulsifying agent dodecyl sodium sulfate 0.09g and 150g mix monomer, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 20 minutes, add 225g mix monomer and 3.71g sodium lauryl sulphate, isothermal reaction 4 hours obtains latex particle size 230nm.
Embodiment nine: prescription: unit (g) Phthalic acid, diallyl ester 370 butyl acrylates 5 Potassium Persulphates 1.2 sodium lauryl sulphate 3.8 water 360
At first in reactor, add emulsifying agent dodecyl sodium sulfate 0.3g and 150g mix monomer, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 15 minutes, add 225g mix monomer and 3.5g sodium lauryl sulphate, isothermal reaction 4 hours obtains latex particle size 469nm.
Embodiment ten: prescription: unit (g) Phthalic acid, diallyl ester 370 butyl acrylates 5 Potassium Persulphates 1.2 sodium lauryl sulphate 3.8 water 360
At first in reactor, add emulsifying agent dodecyl sodium sulfate 0.09g and 150g mix monomer, water 360g, initiator 1.2g, be warming up to 70 ℃ of reactions, react after 18 minutes, add 125g mix monomer and 2.21g sodium lauryl sulphate, react and add 100g mix monomer and 1.5g emulsifying agent after 30 minutes again, isothermal reaction 5 hours obtains latex particle size 250nm.
Claims (7)
1. an esters of acrylic acid latex preparation method is characterized in that 1) add the emulsifying agent account for reaction monomers total amount 0.01-0.09wt% to polymeric kettle; 2) add the reaction monomers that accounts for reaction monomers total amount 30-60wt% to polymeric kettle; 3) add the initiator that accounts for reaction monomers total amount 0.2-0.8wt% to polymeric kettle; 4) add entry to polymeric kettle; Reinforced finishing, add the emulsifying agent that accounts for the monomer of reaction monomers total amount 40-70wt% and account for reaction monomers total amount 0.2-0.8wt% after temperature reaction 15-20 minute again, this partial monosomy and emulsifying agent can be once or gradation add emulsion polymerization systems, reinforced finishing, isothermal reaction 3-5 hour, can make the big particle diameter esters of acrylic acid latex of 200-600nm.
2. preparation method according to claim 1, it is characterized in that described reaction monomers comprise acrylic ester monomer and can with acrylic ester monomer crosslinking copolymerization polymeric monomer.
3. preparation method according to claim 2 is characterized in that described acrylic ester monomer can be methyl acrylate, methyl methacrylate, ethyl propenoate, Jia Jibingxisuanyizhi, butyl acrylate, butyl methacrylate, 2 ethyl hexyl acrylate, Octyl acrylate, Isooctyl acrylate monomer.
4. preparation method according to claim 2 is characterized in that described can be Vinylstyrene, ethylene glycol diacrylate, dimethacrylate second diester, diallyl phthalate with acrylic ester monomer crosslinking copolymerization polymeric monomer.
5. preparation method according to claim 1 is characterized in that described emulsifying agent comprises rosined soap, oleic acid, stearic an alkali metal salt, an alkali metal salt of Witco 1298 Soft Acid, sodium lauryl sulphate, can use separately also and can mix use.
6. preparation method according to claim 5 is characterized in that described emulsifying agent is a sodium lauryl sulphate.
7. preparation method according to claim 1 is characterized in that described initiator comprises Potassium Persulphate, Sodium Persulfate, ammonium persulphate, can be used alone or as a mixture.
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| Application Number | Priority Date | Filing Date | Title |
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| CN00101339A CN1100800C (en) | 2000-01-07 | 2000-01-07 | Synthesis method for large grain size latex |
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| CN00101339A CN1100800C (en) | 2000-01-07 | 2000-01-07 | Synthesis method for large grain size latex |
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| CN1260352A CN1260352A (en) | 2000-07-19 |
| CN1100800C true CN1100800C (en) | 2003-02-05 |
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| CN00101339A Expired - Fee Related CN1100800C (en) | 2000-01-07 | 2000-01-07 | Synthesis method for large grain size latex |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338005B (en) * | 2008-03-11 | 2011-03-30 | 郑勇 | Process for synthesizing acrylic ester copolymer of ultra-high molecular mass |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1123290A (en) * | 1994-11-15 | 1996-05-29 | 奇美实业股份有限公司 | Method for producing thermoplastic styrene resin compound |
| CN1237185A (en) * | 1997-07-29 | 1999-12-01 | 钟渊化学工业株式会社 | Graft copolymer particles and thermoplastic resin compositions |
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- 2000-01-07 CN CN00101339A patent/CN1100800C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1123290A (en) * | 1994-11-15 | 1996-05-29 | 奇美实业股份有限公司 | Method for producing thermoplastic styrene resin compound |
| CN1237185A (en) * | 1997-07-29 | 1999-12-01 | 钟渊化学工业株式会社 | Graft copolymer particles and thermoplastic resin compositions |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338005B (en) * | 2008-03-11 | 2011-03-30 | 郑勇 | Process for synthesizing acrylic ester copolymer of ultra-high molecular mass |
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