CN112851969A - Polymer emulsion and method and apparatus for preparing the same - Google Patents

Polymer emulsion and method and apparatus for preparing the same Download PDF

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Publication number
CN112851969A
CN112851969A CN202110026189.1A CN202110026189A CN112851969A CN 112851969 A CN112851969 A CN 112851969A CN 202110026189 A CN202110026189 A CN 202110026189A CN 112851969 A CN112851969 A CN 112851969A
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stirring
polymer
emulsion
dispersion medium
liquid
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CN112851969B (en
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安曼
焦康
成志秀
赵义丽
许剑
高甲
刘邵帅
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China Lucky Group Corp
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China Lucky Group Corp
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1862—Stationary reactors having moving elements inside placed in series
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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    • C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2371/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
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    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2471/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids

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  • Chemical & Material Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention provides a polymer emulsion and a preparation method and a device thereof. The method for preparing the polymer emulsion comprises the following steps: under the condition of first stirring treatment, mixing a hydrophilic polymer and a hydrophobic polymer to obtain a pre-emulsion; adding a dispersion medium to the pre-emulsion under conditions of a second stirring treatment so as to obtain the polymer emulsion, wherein a second stirring rate of the second stirring treatment is greater than a first stirring rate of the first stirring treatment, and a rate of adding the dispersion medium to the pre-emulsion is not less than 100 kg/s. The method is simple and convenient to operate, easy to realize, easy for industrial production and strong in stability, and particularly can be used for effectively preparing the polymer emulsion with narrow particle size distribution.

Description

Polymer emulsion and method and apparatus for preparing the same
Technical Field
The invention relates to the technical field of chemical engineering, in particular to a polymer emulsion and a preparation method and a device thereof.
Background
The polymer emulsion is a material with excellent performance, wherein the water-based polymer emulsion is also an environment-friendly material and has the advantages of no toxicity, difficult combustion, no environmental pollution and the like. At present, polymer emulsions are widely used in industrial production of coatings, adhesives, leather, textiles, etc., and in the related art, the particle size distribution of polymer emulsions is usually an important index for measuring the quality of polymer emulsions. However, the particle size distribution of the polymer emulsion prepared by the current process is still wide, and the production requirement cannot be met.
Thus, the related art of the existing polymer emulsion still remains to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, an object of the present invention is to provide a method for preparing a polymer emulsion with narrow particle size distribution, which is simple, convenient, easy to implement, easy for industrial production, and strong in stability.
In one aspect of the invention, a method of making a polymer emulsion is provided. According to an embodiment of the invention, the method comprises: under the condition of first stirring treatment, mixing a hydrophilic polymer and a hydrophobic polymer to obtain a pre-emulsion; adding a dispersion medium to the pre-emulsion under conditions of a second stirring treatment so as to obtain the polymer emulsion, wherein a second stirring rate of the second stirring treatment is greater than a first stirring rate of the first stirring treatment, and a rate of adding the dispersion medium to the pre-emulsion is not less than 100 kg/s. The inventor finds that the method is simple and convenient to operate, easy to implement, easy for industrial production and strong in stability, and particularly can be used for effectively preparing the polymer emulsion with narrow particle size distribution.
According to an embodiment of the present invention, the difference between the second stirring rate and the first stirring rate is 500rpm to 2000 rpm.
According to an embodiment of the present invention, the second stirring rate is 1500rpm to 2500rpm, and the first stirring rate is 500rpm to 1000 rpm.
According to an embodiment of the present invention, the first agitation treatment and the second agitation treatment each independently satisfy at least one of the following conditions: the temperature of the first stirring treatment and the temperature of the second stirring treatment are respectively and independently 25-40 ℃; the first stirring time of the first stirring treatment is 30-50 min; and the second stirring time of the second stirring treatment is 15-30 min.
According to an embodiment of the present invention, the step of mixing the hydrophilic polymer and the hydrophobic polymer under the condition of the first agitation treatment to obtain the pre-emulsion is performed by mixing a first solution containing the hydrophilic polymer and a second solution containing the hydrophobic polymer, and after obtaining the polymer emulsion, at least one of the following steps is further included: removing the solvent of the first solution contained in the polymer emulsion; removing the solvent of the second solution contained in the polymer emulsion.
According to an embodiment of the invention, the method satisfies at least one of the following conditions: the hydrophilic polymer comprises at least one of polyvinyl alcohol and polyethylene glycol; the hydrophobic polymer comprises at least one of polyvinylidene fluoride, polytetrafluoroethylene and polyisophthaloyl metaphenylene diamine; the dispersion medium includes at least one of water and an organic dispersion medium.
In another aspect of the invention, the invention provides a polymer emulsion. According to the embodiment of the invention, the polymer emulsion is prepared by the method, and the polymer particles in the polymer emulsion have a core-shell structure and meet any one of the following conditions: (1) the core of the core-shell structure comprises the hydrophilic polymer; the shell of the core-shell structure comprises the hydrophobic polymer; the polymer particles are dispersed in the dispersion medium, and the dispersion medium is an organic dispersion medium; (2) the core of the core-shell structure comprises the hydrophobic polymer; the shell of the core-shell structure comprises the hydrophilic polymer; the polymer particles are dispersed in the dispersion medium, and the dispersion medium is water. The inventor finds that the polymer emulsion has strong stability and narrow particle size distribution.
In a further aspect of the invention, there is provided an apparatus for carrying out the method or for preparing the polymer emulsion described above. According to an embodiment of the invention, the apparatus comprises: a kettle body having an accommodation chamber; a stirring assembly having a stirring portion movably disposed in the receiving chamber; the liquid adding assembly is arranged on one side of the kettle body and is suitable for adding the dispersion medium into the accommodating chamber; and the control assembly is used for controlling the stirring of the stirring assembly and/or the liquid adding of the liquid adding assembly. The inventor finds that the device has simple structure, high automation degree, low cost and easy industrialization, and can effectively implement the method or effectively prepare the polymer emulsion.
According to an embodiment of the invention, the agitator in the agitator assembly is a pitched blade agitator.
According to an embodiment of the invention, the apparatus comprises: the kettle body is provided with the accommodating chamber, the side wall of the accommodating chamber is provided with a feeding hole, and the bottom wall of the accommodating chamber is provided with a discharging hole; the stirring component is provided with a stirring motor, a stirring shaft and a stirrer are arranged on the stirring motor, and the stirring shaft and the stirrer jointly form the stirring part; the liquid feeding assembly comprises a liquid containing tank, the liquid containing tank is connected with the accommodating cavity through a first pipeline, a liquid discharging valve is arranged in the first pipeline, an overflow port and a limit switch are further arranged in the liquid containing tank, and the liquid containing tank is connected with an upper liquid valve through a second pipeline; and the control assembly comprises a programmable logic controller and a control panel, the programmable logic controller is electrically connected with the control panel, the programmable logic controller is used for controlling the stirring of the stirring assembly and/or the liquid adding of the liquid adding assembly, and the control panel is used for receiving control instructions of the stirring and/or the liquid adding.
Drawings
FIG. 1 shows a schematic flow diagram of a method of making a polymer emulsion according to one embodiment of the present invention.
FIG. 2 shows a schematic structural view of an apparatus for preparing a polymer emulsion according to an embodiment of the present invention.
Fig. 3 shows a schematic structural diagram of a programmable logic controller according to an embodiment of the present invention.
Fig. 4 shows a schematic structural diagram of a control panel according to an embodiment of the present invention.
Reference numerals:
1: and (3) kettle body 2: a stirring motor 3: a stirring shaft 4: the stirrer 5: liquid discharge valve 6: a liquid containing tank 7: liquid feeding valve 8: feed inlet 9: a discharge port 10: an overflow port 11: the limit switch 12: first pipe 13: second duct 14: the programmable logic controller 15: panel display and key control module 16: limit switch control module 17: the upper liquid control module 18: the motor control module 19: the tapping control module 20: control panel
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
In one aspect of the invention, a method of making a polymer emulsion is provided. According to an embodiment of the invention, referring to fig. 1, the method may specifically comprise the steps of:
s100: under the condition of the first stirring treatment, the hydrophilic polymer and the hydrophobic polymer are mixed to obtain a pre-emulsion.
S200: adding a dispersion medium to the pre-emulsion under conditions of a second stirring treatment so as to obtain the polymer emulsion, wherein a second stirring rate of the second stirring treatment is greater than a first stirring rate of the first stirring treatment, and a rate of adding the dispersion medium to the pre-emulsion is not less than 100 kg/s.
The inventor finds that the method with the steps is simple and convenient to operate, easy to implement, easy for industrial production and strong in stability, and particularly, the polymer emulsion with narrow particle size distribution can be effectively prepared by the method with the steps.
Further, according to an embodiment of the present invention, the rate of adding the dispersion medium to the pre-emulsion may be specifically 100kg/s, 120kg/s, 140kg/s, 160kg/s, or 180kg/s, or the like. Thus, the rate of addition of the dispersion medium is sufficiently fast that the hydrophobic polymer as described above does not precipitate out, and the particle size distribution of the resulting polymer emulsion can be further narrowed.
According to an embodiment of the present invention, further, a difference between the second stirring rate and the first stirring rate may be 500rpm to 2000 rpm. In particular, in some embodiments of the present invention, the difference between the second stirring rate and the first stirring rate may specifically be 500rpm, 1000rpm, 1500rpm, 2000rpm, or the like. Therefore, the difference between the second stirring speed and the first stirring speed is proper, so that the particle size distribution of the prepared polymer emulsion can be further narrower.
According to embodiments of the present invention, in some more specific embodiments of the present invention, the second stirring rate may be 1500rpm to 2500rpm, and the first stirring rate may be 500rpm to 1000 rpm. Specifically, the second stirring rate may be 1500rpm, 2000rpm, 2500rpm, or the like; the first stirring rate may be 500rpm, 600rpm, 700rpm, 800rpm, 900rpm, 1000rpm, or the like. Therefore, the first stirring speed is proper, and the first stirring speed is not too low to cause insufficient mechanical stirring and not too high to cause liquid splashing; the second stirring rate is also proper, and the second stirring rate is not too low, so that the hydrophobic polymer can be separated out when the dispersion medium is added, and is not too high, so that the reactant can splash, the hydrophobic polymer can be separated out, and the particle size distribution of the prepared polymer emulsion can be further narrower.
According to an embodiment of the present invention, the first agitation treatment and the second agitation treatment may each independently satisfy the following condition: the temperature of the first stirring treatment and the temperature of the second stirring treatment may be each independently 25 to 40 ℃, specifically, 25 ℃, 30 ℃, 35 ℃, or 40 ℃ or the like; the first stirring time of the first stirring treatment may be 30min to 50min, specifically, 30min, 40min, or 50 min; the second stirring time of the second stirring treatment may be 15min to 30min, specifically, 15min, 20min, 25min, 30min, or the like. Therefore, the temperature is not too low, so that the viscosity of the mixed hydrophobic polymer and hydrophilic polymer is too high, the mixed hydrophobic polymer and hydrophilic polymer are not easy to stir and mix uniformly, the solvent is not volatilized due to too high temperature, and the solid content of the mixed solution is increased.
According to an embodiment of the present invention, the step of mixing the hydrophilic polymer and the hydrophobic polymer under the condition of the first agitation treatment to obtain the pre-emulsion is performed by mixing a first solution containing the hydrophilic polymer and a second solution containing the hydrophobic polymer, and after obtaining the polymer emulsion, at least one of the following steps is further included: removing the solvent of the first solution contained in the polymer emulsion; removing the solvent of the second solution contained in the polymer emulsion, wherein a specific process for removing the solvent can be a membrane separation technology, and specific process steps, conditions and parameters of the process can be the same as those of the membrane separation technology in the related technology, and are not described in detail herein; the first solvent and the second solvent may be the same or different; may or may not be miscible with water, and will not be described herein in any greater detail. Therefore, the polymer emulsion with narrow particle size distribution can be further effectively prepared, and the polymer emulsion has strong stability.
According to an embodiment of the invention, further, the method satisfies at least one of the following conditions: the hydrophilic polymer comprises at least one of polyvinyl alcohol and polyethylene glycol; the hydrophobic polymer comprises at least one of polyvinylidene fluoride, polytetrafluoroethylene and polyisophthaloyl metaphenylene diamine; the dispersion medium includes at least one of water and an organic dispersion medium, although it will be understood by those skilled in the art that the hydrophilic polymer may include other hydrophilic polymers having-COOH, -OH, -NH2or-CONH2An isofunctional polymer; the hydrophobic polymer may also include other polymers having functional groups such as-CONH, -F, -Cl, or C ═ O, and thus, the description thereof is not repeated herein. Therefore, the material source is wide and easy to obtain, the cost is low, the hydrophilic polymer emulsion or the hydrophobic polymer emulsion can be effectively prepared, and the application range is wide.
In another aspect of the invention, the invention provides a polymer emulsion. According to the embodiment of the invention, the polymer emulsion is prepared by the method, and the polymer particles in the polymer emulsion have a core-shell structure and meet any one of the following conditions: (1) the core of the core-shell structure comprises the hydrophilic polymer; the shell of the core-shell structure comprises the hydrophobic polymer; the polymer particles are dispersed in the dispersion medium, and the dispersion medium is an organic dispersion medium; (2) the core of the core-shell structure comprises the hydrophobic polymer; the shell of the core-shell structure comprises the hydrophilic polymer; the polymer particles are dispersed in the dispersion medium, and the dispersion medium is water. The inventor finds that the polymer emulsion has strong stability and narrow particle size distribution.
According to an embodiment of the present invention, the polymer particles in the polymer emulsion may be formed by non-covalent bond interactions, wherein the non-covalent bond may include van der waals force, electrostatic attraction, hydrogen bond force, hydrophobic interaction, and the like, and will not be described in detail herein. Therefore, the polymer emulsion has narrow particle size distribution and strong stability.
In a further aspect of the invention, there is provided an apparatus for carrying out the method or for preparing the polymer emulsion described above. According to an embodiment of the invention, the apparatus may comprise: a kettle body having an accommodation chamber; a stirring assembly having a stirring portion movably disposed in the receiving chamber; the liquid adding assembly is arranged on one side of the kettle body and is suitable for adding the dispersion medium into the accommodating chamber; and the control assembly is used for controlling the stirring of the stirring assembly and/or the liquid adding of the liquid adding assembly. The inventor finds that the device has simple structure, high automation degree, low cost and easy industrialization, and can effectively implement the method or effectively prepare the polymer emulsion.
According to an embodiment of the present invention, further, the stirrer in the stirring assembly may be a pitched blade stirrer. Therefore, the stirring process has higher displacement, high circulation rate and lower power consumption.
According to an embodiment of the present invention, further, referring to fig. 2, the apparatus may include: the kettle body 1 is provided with the accommodating chamber, the side wall of the accommodating chamber is provided with a feeding hole 8, and the bottom wall of the accommodating chamber is provided with a discharging hole 9; the stirring component is provided with a stirring motor 2, a stirring shaft 3 and a stirrer 4 are arranged on the stirring motor 2, and the stirring shaft 3 and the stirrer 4 jointly form the stirring part; the liquid adding assembly comprises a liquid containing tank 6, the liquid containing tank 6 is connected with the accommodating chamber through a first pipeline 12, a liquid discharging valve 5 is arranged in the first pipeline 12, an overflow port 10 and a limit switch 11 are further arranged in the liquid containing tank 6, and the liquid containing tank 6 is connected with a liquid feeding valve 7 through a second pipeline 13; and the control assembly comprises a programmable logic controller 14 (with reference to the structural schematic diagram in fig. 3) and a control panel 20 (with reference to the structural schematic diagram in fig. 4), wherein the programmable logic controller 14 is electrically connected with the control panel 20 (not shown in the figure), the programmable logic controller 14 is used for controlling the stirring assembly to stir and/or the liquid adding assembly to add liquid, and the control panel is used for receiving control commands of the stirring assembly and/or the liquid adding assembly to add liquid.
According to the embodiment of the present invention, specifically, the kettle body 1 may be provided with a jacket, so as to allow a cooling medium or a heating medium to pass through; the liquid discharging valve 5 can be a pneumatic butterfly valve and is provided with an electromagnetic valve fitting, and the opening or closing of the pneumatic butterfly valve is controlled by controlling the electromagnetic valve through the programmable logic controller 14; the liquid feeding valve 7 can be an electromagnetic valve, one end of the liquid feeding valve is connected with the liquid containing tank 6 through a second pipeline 13, and the other end of the liquid feeding valve is connected with the liquid inlet pipe.
According to an embodiment of the present invention, specifically, the programmable logic controller 14 may specifically include a panel display and key control module 15, a limit switch control module 16, a liquid feeding control module 17, a motor control module 18, and a liquid discharging control module 19 (the structural schematic diagram refers to fig. 3); the programmable logic controller 14 may be of the type siemens S7-200; the panel display and key control module 15 is connected with a control panel 20 (not shown in the figure) and is used for panel display, setting of equipment parameters and control of operating keys; the control panel 20 may be a touch screen; the limit switch control module 16 may be connected to the limit switch 11 (not shown in the figure), and stops adding when the amount of the dispersion medium reaches the position set by the limit switch, so as to control the amount of the dispersion medium added in the manufacturing process of the emulsion polymer; the upper liquid control module 17 can be connected with the upper liquid valve 7 (not shown in the figure) and is used for controlling the opening and closing of the upper liquid valve 7 so as to realize the quantitative addition of the dispersion medium; the motor control module 18 can be connected with the stirring motor 2 (not shown in the figure), and the input frequency of the stirring motor 2 is controlled so as to change the stirring rotating speed; the tapping control module 19 is connected to the tapping valve 5 (not shown in the drawings) for controlling the opening and closing of the tapping valve 5 so as to rapidly add the dispersion medium to the vessel 1 in a short time.
Specifically, in one particular embodiment of the invention, the device is used by: hydrophilic polymer and hydrophobic polymer are respectively added into the kettle body 1 through the feed inlet 8, after the addition is completed, preparation parameters including temperature, stirring speed and stirring time are set through the control panel 20, the parameters are started after the setting is completed, and the stirring motor 2 drives the stirring shaft 3 and the stirrer 4 to rotate and shear, so that the hydrophilic polymer and the hydrophobic polymer are fully stirred and uniformly mixed. Meanwhile, the upper liquid valve 7 is opened, the liquid inlet pipe adds water to the liquid containing tank 6 through the pipeline 13, and when the water level reaches the limit switch 11, the upper liquid valve 7 is closed, and the water adding is stopped. When the mixing and stirring time is up, the programmable logic controller 14 increases the stirring rotating speed by changing the input frequency of the stirring motor 2, when the stirring rotating speed reaches a preset value, the tapping valve 5 is opened, water in the liquid containing tank 6 is rapidly added into the kettle body 1 through the first pipeline 12, and the tapping valve 5 is closed. Stirring for a certain time to obtain polymer emulsion, and further, conveying the polymer emulsion to a membrane separation system device through a discharge port 9 to remove the solvent in the polymer emulsion. Therefore, the method is simple and convenient to operate, easy to realize and easy for industrial production.
The following describes embodiments of the present invention in detail.
Example 1
Mixing a polyvinylidene fluoride solution (the solvent is dimethylformamide) and a polyvinyl alcohol solution (the solvent is dimethylformamide) for 30min under the conditions that the temperature is 25 ℃ and the first stirring speed is 500rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 2500rpm, so as to obtain the polymer emulsion, wherein after the water is added to the pre-emulsion at a rate of 120kg/s, stirring is continued for 15min after the water is added.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Example 2
Mixing a polyvinylidene fluoride solution (solvent dimethylacetamide) and a polyvinyl alcohol solution (solvent dimethylacetamide) for 40min under the conditions that the temperature is 30 ℃ and the first stirring speed is 750rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 1500rpm to obtain the polymer emulsion, wherein after adding the water to the pre-emulsion at a rate of 120kg/s, stirring is continued for 20min after adding the water.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Example 3
Mixing a polytetrafluoroethylene solution (solvent dimethylacetamide) and a polyvinyl alcohol solution (solvent dimethylacetamide) for 45min under the conditions that the temperature is 30 ℃ and the first stirring speed is 1000rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 2000rpm, so as to obtain the polymer emulsion, wherein after adding the water to the pre-emulsion at a rate of 130kg/s, stirring is continued for 20min after adding the water.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Example 4
Mixing a polyvinylidene fluoride solution (solvent dimethylformamide) and a polyethylene glycol solution (solvent dimethylformamide) for 50min under the conditions that the temperature is 40 ℃ and the first stirring speed is 1000rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 2000rpm, so as to obtain the polymer emulsion, wherein after the water is added to the pre-emulsion at a rate of 100kg/s, stirring is continued for 30min after the water is added.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Example 5
Mixing a polyisophthaloyl metaphenylene diamine solution (solvent dimethylformamide) and a polyethylene glycol solution (solvent dimethylformamide) for 30min under the conditions that the temperature is 35 ℃ and the first stirring speed is 1000rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 1800rpm, so as to obtain the polymer emulsion, wherein after the water is added to the pre-emulsion at a rate of 120kg/s, stirring is continued for 30min after the water is added.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Comparative example 1
Mixing a polytetrafluoroethylene solution (solvent dimethylacetamide) and a polyethylene glycol solution (solvent dimethylacetamide) for 20min under the conditions that the temperature is 30 ℃ and the first stirring speed is 500rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 750rpm, so as to obtain the polymer emulsion, wherein after the water is added to the pre-emulsion at a rate of 100kg/s, stirring is continued for 20min after the water is added.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Comparative example 2
Mixing a polyvinylidene fluoride solution (solvent dimethylacetamide) and a polyvinyl alcohol solution (solvent dimethylacetamide) for 15min under the conditions that the temperature is 15 ℃ and the first stirring speed is 500rpm to obtain a pre-emulsion;
adding water to the pre-emulsion at a temperature of 25 ℃ and a second stirring rate of 1500rpm to obtain the polymer emulsion, wherein after adding the water to the pre-emulsion at a rate of 60kg/s, stirring is continued for 20min after adding the water.
Finally, the solvent is removed by adopting a membrane separation technology to prepare the polymer emulsion.
The polymer emulsion was tested for particle size distribution and the results are shown in Table 1.
Table 1 results of particle size distribution test of examples 1 to 5, comparative example 1, and comparative example 2
Example 1 Example 2 Example 3 Example 4 Example 5 Comparative example 1 Comparative example 2
D10(μm) 0.314 0.315 0.283 0.315 0.318 0.330 0.323
D50(μm) 0.559 0.571 0.585 0.590 0.604 0.716 0.629
D90(μm) 4.167 3.979 4.205 4.300 4.761 35.06 21.00
Span of 6.882 6.406 6.701 6.744 7.349 48.47 26.96
As can be seen from Table 1, the process with the steps described in the present invention can efficiently produce polymer emulsions with narrow particle size distributions.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. A method of making a polymer emulsion, comprising:
under the condition of first stirring treatment, mixing a hydrophilic polymer and a hydrophobic polymer to obtain a pre-emulsion;
adding a dispersion medium to the pre-emulsion under conditions of a second agitation treatment so as to obtain the polymer emulsion,
wherein the second stirring rate of the second stirring treatment is greater than the first stirring rate of the first stirring treatment, and the rate of adding the dispersion medium to the pre-emulsion is not less than 100 kg/s.
2. The method of claim 1, wherein the difference between the second stirring rate and the first stirring rate is 500rpm to 2000 rpm.
3. The method of claim 2, wherein the second stirring rate is 1500rpm to 2500rpm and the first stirring rate is 500rpm to 1000 rpm.
4. The method according to claim 3, wherein the first agitation treatment and the second agitation treatment each independently satisfy at least one of the following conditions:
the temperature of the first stirring treatment and the temperature of the second stirring treatment are respectively and independently 25-40 ℃;
the first stirring time of the first stirring treatment is 30-50 min;
and the second stirring time of the second stirring treatment is 15-30 min.
5. The method of claim 1, wherein the step of mixing the hydrophilic polymer and the hydrophobic polymer under the first agitation treatment to obtain the pre-emulsion is performed by mixing a first solution containing the hydrophilic polymer and a second solution containing the hydrophobic polymer, and further comprises at least one of the following steps after obtaining the polymer emulsion:
removing the solvent of the first solution contained in the polymer emulsion;
removing the solvent of the second solution contained in the polymer emulsion.
6. The method of claim 1, wherein at least one of the following conditions is satisfied:
the hydrophilic polymer comprises at least one of polyvinyl alcohol and polyethylene glycol;
the hydrophobic polymer comprises at least one of polyvinylidene fluoride, polytetrafluoroethylene and polyisophthaloyl metaphenylene diamine;
the dispersion medium includes at least one of water and an organic dispersion medium.
7. A polymer emulsion prepared by the method of any one of claims 1 to 6, wherein the polymer particles in the polymer emulsion have a core-shell structure and satisfy any one of the following conditions:
(1) the core of the core-shell structure comprises the hydrophilic polymer; the shell of the core-shell structure comprises the hydrophobic polymer; the polymer particles are dispersed in the dispersion medium, and the dispersion medium is an organic dispersion medium;
(2) the core of the core-shell structure comprises the hydrophobic polymer; the shell of the core-shell structure comprises the hydrophilic polymer; the polymer particles are dispersed in the dispersion medium, and the dispersion medium is water.
8. An apparatus for carrying out the process according to any one of claims 1 to 6 or for preparing the polymer emulsion according to claim 7, comprising:
a kettle body having an accommodation chamber;
a stirring assembly having a stirring portion movably disposed in the receiving chamber;
the liquid adding assembly is arranged on one side of the kettle body and is suitable for adding the dispersion medium into the accommodating chamber; and
the control assembly is used for controlling the stirring of the stirring assembly and/or the liquid adding of the liquid adding assembly.
9. The apparatus of claim 8, wherein the agitator in the agitator assembly is a pitched blade agitator.
10. The apparatus of claim 8, comprising:
the kettle body is provided with the accommodating chamber, the side wall of the accommodating chamber is provided with a feeding hole, and the bottom wall of the accommodating chamber is provided with a discharging hole;
the stirring component is provided with a stirring motor, a stirring shaft and a stirrer are arranged on the stirring motor, and the stirring shaft and the stirrer jointly form the stirring part;
the liquid feeding assembly comprises a liquid containing tank, the liquid containing tank is connected with the accommodating cavity through a first pipeline, a liquid discharging valve is arranged in the first pipeline, an overflow port and a limit switch are further arranged in the liquid containing tank, and the liquid containing tank is connected with an upper liquid valve through a second pipeline; and
the control assembly comprises a programmable logic controller and a control panel, the programmable logic controller is electrically connected with the control panel, the programmable logic controller is used for controlling the stirring of the stirring assembly and/or the liquid adding of the liquid adding assembly, and the control panel is used for receiving control instructions of the stirring and/or the liquid adding.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103599714A (en) * 2013-09-27 2014-02-26 神华集团有限责任公司 Dispersive droplet emulsion and preparation method thereof
CN105017750A (en) * 2014-04-28 2015-11-04 乐凯胶片股份有限公司 Water-based aromatic polyamide emulsion, preparation method and application of water-based aromatic polyamide emulsion
CN205035322U (en) * 2015-08-13 2016-02-17 宁波大学 Pitch emulsification reaction kettle
CN208554198U (en) * 2018-07-06 2019-03-01 成都德美精英化工有限公司 A kind of emulsion polymerization device
CN208679137U (en) * 2018-06-06 2019-04-02 浙江中科立德新材料有限公司 A kind of full-automatic lotion production reaction kettle
CN109988322A (en) * 2019-02-21 2019-07-09 中国乐凯集团有限公司 Water-based fluoropolymer emulsion, preparation method and applications

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103599714A (en) * 2013-09-27 2014-02-26 神华集团有限责任公司 Dispersive droplet emulsion and preparation method thereof
CN105017750A (en) * 2014-04-28 2015-11-04 乐凯胶片股份有限公司 Water-based aromatic polyamide emulsion, preparation method and application of water-based aromatic polyamide emulsion
CN205035322U (en) * 2015-08-13 2016-02-17 宁波大学 Pitch emulsification reaction kettle
CN208679137U (en) * 2018-06-06 2019-04-02 浙江中科立德新材料有限公司 A kind of full-automatic lotion production reaction kettle
CN208554198U (en) * 2018-07-06 2019-03-01 成都德美精英化工有限公司 A kind of emulsion polymerization device
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