CN113307987A - Preparation method of brominated butyl rubber latex - Google Patents

Preparation method of brominated butyl rubber latex Download PDF

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CN113307987A
CN113307987A CN202110575540.2A CN202110575540A CN113307987A CN 113307987 A CN113307987 A CN 113307987A CN 202110575540 A CN202110575540 A CN 202110575540A CN 113307987 A CN113307987 A CN 113307987A
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emulsifier
butyl rubber
latex
brominated butyl
shearing
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周元林
李迎军
李银涛
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Southwest University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/07Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
    • AHUMAN NECESSITIES
    • A41WEARING APPAREL
    • A41DOUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D19/00Gloves
    • A41D19/0055Plastic or rubber gloves
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/26Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
    • C08L23/28Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
    • C08L23/283Halogenated homo- or copolymers of iso-olefins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/26Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
    • C08J2323/28Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds

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  • General Chemical & Material Sciences (AREA)
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  • Textile Engineering (AREA)
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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a preparation method of brominated butyl rubber latex, which comprises the following steps: dissolving brominated butyl rubber in an organic solvent at 50-60 ℃ to prepare a glue solution, adding an anionic emulsifier, a nonionic emulsifier and a stabilizer into deionized water to prepare an emulsifier aqueous solution; regulating the pH value of the emulsifier aqueous solution by using potassium hydroxide or potassium dihydrogen phosphate; adding the glue solution into an emulsifier aqueous solution, pumping into an emulsification tank, shearing by using a shearing machine, and then performing high shearing action at a certain shearing linear speed to prepare O/W type brominated butyl rubber emulsion; pumping the brominated butyl rubber emulsion into an evaporation kettle, distilling to recover the organic solvent, and obtaining dilute latex with the solid content of 8-15% after distillation is finished; and (4) evaporating and concentrating the dilute latex in an evaporation kettle to obtain latex with certain solid content. The preparation process and flow of the invention are simple and convenient, and can be used for large-scale production, and the prepared latex can widen the application field of the brominated butyl rubber.

Description

Preparation method of brominated butyl rubber latex
The application is a divisional application of Chinese patent application with application number 201610587667.5 and invented name of 'a preparation method of brominated butyl rubber latex' filed by the Chinese patent office on 2016, 07, 25.
Technical Field
The invention belongs to the technical field of rubber latex preparation, and particularly relates to a preparation method of brominated butyl rubber latex.
Background
The brominated butyl rubber is a brominated modified product of butyl rubber, has a highly saturated polyisobutylene main chain of the butyl rubber, and therefore has all the inherent properties of the butyl rubber, such as shock absorption, low glass transition temperature, low permeability of gas and moisture, heat resistance, ozone resistance, ultraviolet irradiation resistance, corrosion resistance and the like; meanwhile, the C-Br bond energy is less than the C-C bond energy, so that the brominated butyl rubber has wide vulcanization conditions, higher vulcanization speed and higher vulcanization flexibility, and has better co-vulcanization performance with the blended rubber. However, the research on the processing of the brominated butyl rubber is mainly a dry rubber processing technology, the process flow and equipment are complex, the ingredients are not uniformly dispersed, certain influence is caused on the product performance, and the realization of linkage and automation is difficult; the production costs are generally high.
The brominated butyl rubber is made into latex, so that the problems can be well solved. For example, chinese patent publication No. CN 101935401 a provides a method for preparing a brominated butyl rubber emulsion. The method adopts the emulsifying strength of 10000 rpm-25000 rpm to prepare the brominated butyl rubber emulsion with the average particle size of 0.7-3.0 mu m. However, the method has large loss of rubber molecular weight in the preparation process. This aspect may be due to improper emulsification processes; on the other hand, when the concentration of the emulsifier is low and the oil-water ratio is high, a higher shearing speed is needed for preparing the aqueous latex with smaller average particle size, and the chain breaking of a molecular chain is easily caused by the action of high shearing force, so that the loss of the molecular weight of the polymer in the emulsification process is high finally. Meanwhile, the latex prepared by the preparation method has a large residual value of the organic solvent, is low in stability and generates a layering phenomenon within 12 hours. At present, the stability of the brominated butyl rubber is rarely studied at home and abroad.
Disclosure of Invention
The invention aims to provide a preparation method of brominated butyl rubber latex, which can reduce the loss of rubber molecules and reduce the residual value of organic solvent; meanwhile, the prepared brominated butyl rubber latex has higher stability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of brominated butyl rubber latex, which comprises the following steps:
dissolving brominated butyl rubber in an organic solvent at 50-60 ℃ for 2-6 h, and preparing glue solution with the concentration of 8-15%;
adding an anionic emulsifier, a nonionic emulsifier and a stabilizer into deionized water to prepare an emulsifier aqueous solution, and adjusting the pH value of the emulsifier aqueous solution to 10.0-12.0 by using potassium hydroxide or potassium dihydrogen phosphate;
adding the glue solution into the emulsifier aqueous solution according to the oil-water ratio of 0.5-1.5, pumping into an emulsification tank, and performing high shearing by using a shearing machine to prepare O/W type brominated butyl rubber emulsion;
the process of high shearing by using the shearing machine comprises the following steps: shearing for 10-30 min under the condition that the shearing linear speed is 1-5 m/s, and then shearing for 0.5-2 h under the condition that the shearing linear speed is 5-15 m/s;
pumping the O/W type brominated butyl rubber emulsion into an evaporation kettle, distilling and recovering the organic solvent, and obtaining dilute latex with the solid content of 8-15% after recovery;
the temperature of the distillation recovery is 30-60 ℃, the vacuum degree is 50-80 kPa, and the time is 3-6 h;
fourthly, evaporating and concentrating the dilute latex through an evaporation kettle to obtain concentrated latex with the solid content of 40-60% and the average particle size of 0.1-2.0 microns;
and step five, preparing the concentrated latex.
Preferably, in the emulsifier aqueous solution, the concentration of the anionic emulsifier is 1.0-5.0%, the concentration of the nonionic emulsifier is 0.2-2.0%, and the concentration of the stabilizer is 0.05-1.0%.
Preferably, the anionic emulsifier is a compound of 12-20 carbon chain alkylbenzene sulfonate, rosin soap, sodium alkyl sulfate, isomeric alcohol ether carboxylate, sodium oleate, potassium oleate and sodium laurate;
the non-ionic emulsifier is a compound of Tween65, Tween81, Tween85, peregal O-20, polyoxyethylene monostearate and octyl phenyl polyoxyethylene ether;
the stabilizer is a compound of monopotassium phosphate, sodium sulfate, potassium laurate, casein and polyethylene glycol.
Preferably, the mass fraction ratio of the anionic emulsifier to the nonionic emulsifier is 1: 1-3: 1.
Preferably, the total dosage of the anionic emulsifier and the nonionic emulsifier is 10-20% of the mass of the dry glue.
Preferably, the evaporation concentration in the fourth step is carried out at the temperature of 50-90 ℃ and the rotating speed of 100-300 rpm.
According to the preparation method of the brominated butyl rubber latex, the anionic emulsifier and the nonionic emulsifier are compounded, and then the latex with low polymer molecular weight loss and high stability is prepared through a certain emulsification process under the action of the stabilizer; the particle size of the latex is 0.1-2.0 μm. The preparation method has simple preparation process and flow and can be used for large-scale production; the prepared latex can be used for manufacturing products with complex shapes and difficult forming, such as gloves, and the like, thereby widening the application field of the brominated butyl rubber.
The total dosage of the emulsifier is only 10-20% of the mass of the dry glue; the molecular weight loss of the polymer in the latex is less than 5.0 percent by adopting an emulsification mode of gradually increasing the shearing linear velocity; the reduced pressure distillation mode is adopted, so that the residual quantity of organic dissolution in the latex can be reduced; by adjusting the formula and optimizing the process, the stability of the latex can be improved, the time for no delamination of the latex is more than 24h, and the mechanical stability of the latex is more than 400 s.
Drawings
FIG. 1 is a flow chart of a method for preparing a brominated butyl rubber latex according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
According to the invention, the brominated butyl rubber latex with high stability is prepared by adjusting the dosage of the emulsifier and other additives and optimizing the process, so that the problems of high processing difficulty, expensive processing equipment and the like of the brominated butyl rubber and high production cost can be solved, and the application range of the brominated butyl rubber is expanded.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
As shown in fig. 1, the preparation method of the brominated butyl rubber latex of the embodiment of the present invention comprises the following steps:
s101: dissolving brominated butyl rubber in an organic solvent at 50-60 ℃ for 2-6 h to prepare a glue solution with the concentration of 8-15%;
adding an anionic emulsifier, a nonionic emulsifier and a stabilizer into deionized water to prepare an emulsifier aqueous solution, wherein the concentration of the anionic emulsifier is preferably 1.0-5.0%, the concentration of the nonionic emulsifier is preferably 0.2-2.0%, the concentration of the stabilizer is preferably 0.05-1.0%, and then adjusting the pH value of the emulsifier aqueous solution to 10.0-12.0 by using potassium hydroxide or potassium dihydrogen phosphate;
s102: adding the glue solution into the emulsifier aqueous solution according to the oil-water ratio of 0.5-1.5, pumping into an emulsification tank, and performing high shearing by using a shearing machine to prepare O/W type brominated butyl rubber emulsion; the process of high shearing by using the shearing machine comprises the following steps: shearing for 10-30 min under the condition that the shearing linear speed is 1-5 m/s, and then shearing for 0.5-2 h under the condition that the shearing linear speed is 5-15 m/s;
s103: pumping the O/W type brominated butyl rubber emulsion into an evaporation kettle, recovering the organic solvent, and obtaining dilute latex with the solid content of 8-15% after the recovery is finished; the organic solvent is recovered by distillation; the temperature of the distillation recovery is 30-60 ℃, the vacuum degree is 50-80 kPa, and the time is 3-6 h; the residual value of the solvent in the brominated butyl rubber emulsion is less than 90mmp, and the loss of the molecular weight is less than 5%;
s104: evaporating and concentrating the dilute latex through an evaporation kettle to obtain concentrated latex with the solid content of 40-60% and the average particle size of 0.1-2.0 microns; the evaporation concentration is carried out under the conditions that the temperature is preferably 50-90 ℃ and the rotating speed is preferably 100-300 rpm;
s105: the concentrated latex is prepared into a certain solid content, and the mechanical stability is more than 400 s.
In the present invention, the anionic emulsifier is preferably a compound of 12-20 carbon chain alkylbenzene sulfonate, rosin soap, sodium alkyl sulfate, isomeric alcohol ether carboxylate, sodium oleate, potassium oleate and sodium laurate;
in the present invention, the non-ionic emulsifier is preferably a complex of Tween65, Tween81, Tween85, peregal O-20, polyoxyethylene monostearate and octylphenyl polyoxyethylene ether;
in the present invention, the stabilizer is preferably a complex of potassium dihydrogen phosphate, sodium sulfate, potassium laurate, casein and polyethylene glycol;
in the invention, the mass fraction ratio of the anionic emulsifier to the nonionic emulsifier is preferably 1: 1-3: 1; the total dosage of the anionic emulsifier and the nonionic emulsifier is preferably 10-20% of the dry glue mass.
In the invention, the O/W type polymer emulsion is prepared by emulsifying in a shearing mode of gradually increasing the shearing linear velocity, so that the molecular weight is less than 5 percent.
In the invention, the pH values of the emulsifier aqueous solution and the latex are preferably 10-12.
The application of the principles of the present invention will now be described in further detail with reference to specific embodiments.
Example 1
1000 parts of glue solution with the concentration of 10 percent of brominated butyl rubber solution are taken and added into emulsifier aqueous solution consisting of 1000 parts of sodium octadecyl benzene sulfonate, rosin soap, peregal O-20 and polyoxyethylene ether, wherein the concentration of an anionic emulsifier is 1.6 percent, the concentration of a nonionic emulsifier is 0.6 percent, the concentration of a stabilizer consisting of potassium dihydrogen phosphate and sodium sulfate is 0.06 percent, and the pH value of the emulsifier aqueous solution is adjusted to be 11 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, firstly carrying out shearing emulsification for 10min at a linear velocity of 3m/s, and then carrying out emulsification for 60min at a linear velocity of 15m/s to obtain the O/W type emulsion. Pumping into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 70 ℃, the distillation time is 3h, and the vacuum degree is 50kPa, and obtaining the dilute latex with the residual value of the organic solvent of 80 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 90 ℃, the concentration time is 6h, and the concentrated latex with the particle size of 1.51 microns, the solid content of 45 percent and the pH value of 11 is obtained.
Taking a certain amount of dilute latex, washing with deionized water to break emulsion, putting into a vacuum drying oven at 40 ℃ for drying for 24h, taking out to determine the loss of the molecular weight of the polymer, wherein the loss rate is 4.2%.
The mechanical stability of the latex is determined to be greater than 400s, with reference to the test standard GB/T8301-2008.
Example 2
1000 parts of glue solution with 9 percent of brominated butyl rubber solution is taken and added into 900 parts of emulsifier aqueous solution consisting of sodium oleate, potassium oleate, sodium laurate, Tween85 and polyoxyethylene ether, wherein the concentration of anionic emulsifier is 2.6 percent, the concentration of nonionic emulsifier is 1 percent, the concentration of stabilizer consisting of potassium dihydrogen phosphate and sodium sulfate is 0.06 percent, and the pH value of the emulsifier aqueous solution is adjusted to be 11 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, emulsifying for 20min by shearing at a linear speed of 2m/s, and emulsifying for 60min at a linear speed of 16m/s to obtain O/W type emulsion. Pumping into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 70 ℃, the distillation time is 3h, and the vacuum degree is 50kPa, and obtaining the dilute latex with the residual value of the organic solvent of 90 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 90 ℃, the concentration time is 6h, and the concentrated latex with the particle size of 1.32 microns, the solid content of 43 percent and the pH value of 11 is obtained.
The loss of molecular weight of the polymer in the latex and the stability of the latex were determined as in example 1, with a loss of 4.5% and a mechanical stability of greater than 400 s.
Example 3
1000 parts of glue solution with the concentration of 10.5 percent of brominated butyl rubber solution is taken and added into emulsifier aqueous solution consisting of 900 parts of sodium hexadecylbenzene sulfonate, sodium oleate, peregal O-20 and Tween65, wherein the concentration of an anionic emulsifier is 2.0 percent, the concentration of a nonionic emulsifier is 0.8 percent, the concentration of a stabilizer consisting of potassium dihydrogen phosphate, casein and polyethylene glycol is 0.08 percent, and the pH value of the emulsifier aqueous solution is adjusted to be 11 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, emulsifying for 20min by shearing at a linear speed of 3m/s, and emulsifying for 90min at a linear speed of 13m/s to obtain O/W type emulsion. Pumping the mixture into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 70 percent, the distillation time is 3 hours, and the vacuum degree is 60kPa, thus obtaining the dilute latex with the residual value of the organic solvent of 70 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 90%, the concentration time is 6h, and the concentrated latex with the particle size of 1.81 microns, the solid content of 48% and the pH value of 12 is obtained.
The loss of molecular weight of the polymer in the latex and the stability of the latex were measured in the same manner as in example 1, giving a loss of 4.1% and a mechanical stability of greater than 400 s.
Example 4
1000 parts of glue solution with the concentration of 11 percent of brominated butyl rubber solution is taken and added into 1200 parts of emulsifier aqueous solution consisting of sodium dodecyl benzene sulfonate, potassium oleate, Tween85 and polyoxyethylene ether, wherein the concentration of anionic emulsifier is 3.0 percent, the concentration of nonionic emulsifier is 1.5 percent, the concentration of stabilizer consisting of casein and polyethylene glycol is 0.2 percent, and the pH value of the emulsifier aqueous solution is adjusted to 10 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, emulsifying for 20min by shearing at a linear speed of 2m/s, and emulsifying for 90min at a linear speed of 15m/s to obtain O/W type emulsion. Pumping into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 40 ℃, the distillation time is 4h, and the vacuum degree is 70kPa, and obtaining the dilute latex with the residual value of the organic solvent of 75 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 85 ℃, the concentration time is 6h, and the concentrated latex with the particle size of 1.61 microns, the solid content of 46 percent and the pH value of 12 is obtained.
The loss of molecular weight of the polymer in the latex and the stability of the latex were measured in the same manner as in example 1, giving a loss of 4.3% and a mechanical stability of greater than 400 s.
Example 5
1000 parts of glue solution with the concentration of 13 percent of brominated butyl rubber solution is taken and added into 1500 parts of emulsifier aqueous solution consisting of sodium hexadecyl sulfate, sodium oleate, peregal O-20 and polyoxyethylene ether, wherein the concentration of an anionic emulsifier is 4.0 percent, the concentration of a nonionic emulsifier is 1.6 percent, the concentrations of monopotassium phosphate and polyethylene glycol stabilizer are 0.8 percent, and the pH value of the emulsifier aqueous solution is adjusted to be 11 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, emulsifying for 20min by shearing at a linear speed of 5m/s, and emulsifying for 80min at a linear speed of 13m/s to obtain O/W type emulsion. Pumping the mixture into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 50 ℃, the distilling time is 5h, and the vacuum degree is 60kPa, and obtaining the dilute latex with the residual value of the organic solvent of 60 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 90 ℃, the concentration time is 6h, and the concentrated latex with the particle size of 1.51 microns, the solid content of 46 percent and the pH value of 12 is obtained.
The loss of molecular weight of the polymer in the latex and the stability of the latex were measured in the same manner as in example 1, giving a loss of 4.6% and a mechanical stability of greater than 400 s.
Example 6
1000 parts of a glue solution with the concentration of a brominated butyl rubber solution of 15 percent are taken and added into an emulsifier aqueous solution consisting of 1800 parts of sodium dodecyl sulfate, sodium oleate, peregal O-20 and polyoxyethylene ether, wherein the concentration of an anionic emulsifier is 4.5 percent, the concentration of a nonionic emulsifier is 1.8 percent, the concentration of potassium laurate and a polyethylene glycol stabilizer is 0.8 percent, and the pH value of the emulsifier aqueous solution is adjusted to be 11 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, firstly carrying out shearing emulsification for 30min at a linear velocity of 5m/s, and then carrying out emulsification for 100min at a linear velocity of 14m/s to obtain the O/W type emulsion. Pumping into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 50 ℃, the distillation time is 5h, and the vacuum degree is 70kPa, and obtaining the dilute latex with the residual value of the organic solvent of 65 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 90 ℃, the concentration time is 6h, and the concentrated latex with the particle size of 1.21 microns, the solid content of 49 percent and the pH value of 12 is obtained.
The loss of molecular weight of the polymer in the latex and the stability of the latex were determined in the same manner as in example 1, giving a loss of 4.8% and a mechanical stability of greater than 400 s.
Example 7
1000 parts of glue solution with the concentration of 8 percent of brominated butyl rubber solution is taken and added into an emulsifier aqueous solution consisting of 800 parts of sodium hexadecylsulfate, sodium oleate, peregal O-20 and polyoxyethylene ether, wherein the concentration of an anionic emulsifier is 4 percent, the concentration of a nonionic emulsifier is 1.5 percent, the concentration of a stabilizer consisting of monopotassium phosphate, polyethylene glycol and potassium laurate is 0.6 percent, and the pH value of the emulsifier aqueous solution is adjusted to be 11 by potassium hydroxide. Pumping the emulsifier and the glue solution into an emulsification tank by a pump, firstly carrying out shearing emulsification for 30min at a linear velocity of 5m/s, and then carrying out emulsification for 60min at a linear velocity of 14m/s to obtain the O/W type emulsion. Pumping the mixture into an evaporation kettle for distilling to remove the organic solvent, wherein the emulsion temperature is 50 ℃, the distilling time is 3h, and the vacuum degree is 55kPa, and obtaining the dilute latex with the residual value of the organic solvent of 68 ppm. Concentrating by adopting an evaporation concentration mode, wherein the temperature of the latex is 90 ℃, the concentration time is 5h, and the concentrated latex with the particle size of 1.71 microns, the solid content of 46 percent and the pH value of 12 is obtained.
The loss of molecular weight of the polymer in the latex and the stability of the latex were measured in the same manner as in example 1, giving a loss of 4.6% and a mechanical stability of greater than 400 s.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (6)

1. A preparation method of brominated butyl rubber latex is characterized by comprising the following steps:
dissolving brominated butyl rubber in an organic solvent at 50-60 ℃ for 2-6 h, and preparing glue solution with the concentration of 8-15%;
adding an anionic emulsifier, a nonionic emulsifier and a stabilizer into deionized water to prepare an emulsifier aqueous solution, and adjusting the pH value of the emulsifier aqueous solution to 10.0-12.0 by using potassium hydroxide or potassium dihydrogen phosphate;
adding the glue solution into the emulsifier aqueous solution according to the oil-water ratio of 0.5-1.5, pumping into an emulsification tank, and performing high shearing by using a shearing machine to prepare O/W type brominated butyl rubber emulsion;
the process of high shearing by using the shearing machine comprises the following steps: shearing for 10-30 min under the condition that the shearing linear speed is 1-5 m/s, and then shearing for 0.5-2 h under the condition that the shearing linear speed is 5-15 m/s;
pumping the O/W type brominated butyl rubber emulsion into an evaporation kettle, distilling and recovering the organic solvent, and obtaining dilute latex with the solid content of 8-15% after recovery;
the temperature of the distillation recovery is 30-60 ℃, the vacuum degree is 50-80 kPa, and the time is 3-6 h;
fourthly, evaporating and concentrating the dilute latex through an evaporation kettle to obtain concentrated latex with the solid content of 40-60% and the average particle size of 0.1-2.0 microns;
and step five, preparing the concentrated latex to obtain the brominated butyl rubber latex.
2. The method for producing a brominated butyl rubber latex according to claim 1, wherein the aqueous emulsifier solution has a concentration of 1.0% to 5.0% of an anionic emulsifier, a concentration of 0.2% to 2.0% of a nonionic emulsifier, and a concentration of 0.05% to 1.0% of a stabilizer.
3. The method of preparing a brominated butyl rubber latex according to claim 2, wherein the anionic emulsifier is a complex of 12-20 carbon chain alkylbenzene sulfonates, rosin soaps, sodium alkyl sulfates, isomeric alcohol ether carboxylates, sodium oleate, potassium oleate and sodium laurate;
the non-ionic emulsifier is a compound of Tween65, Tween81, Tween85, peregal O-20, polyoxyethylene monostearate and octyl phenyl polyoxyethylene ether;
the stabilizer is a compound of monopotassium phosphate, sodium sulfate, potassium laurate, casein and polyethylene glycol.
4. The method according to claim 2 or 3, wherein the mass fraction ratio of the anionic emulsifier to the nonionic emulsifier is 1:1 to 3: 1.
5. The method according to claim 4, wherein the total amount of the anionic emulsifier and the nonionic emulsifier is 10 to 20% by mass of the dry glue.
6. The method for preparing brominated butyl rubber latex according to claim 1, wherein the evaporation and concentration in the fourth step are carried out at a temperature of 50 to 90 ℃ and a rotation speed of 100 to 300 rpm.
CN202110575540.2A 2016-07-25 2016-07-25 Preparation method of brominated butyl rubber latex Pending CN113307987A (en)

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