CN108285539B - Cationic polymer emulsifying wax and preparation method thereof - Google Patents
Cationic polymer emulsifying wax and preparation method thereof Download PDFInfo
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- CN108285539B CN108285539B CN201810066673.5A CN201810066673A CN108285539B CN 108285539 B CN108285539 B CN 108285539B CN 201810066673 A CN201810066673 A CN 201810066673A CN 108285539 B CN108285539 B CN 108285539B
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
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- C08J2391/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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- C08J2433/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2433/14—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
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Abstract
The invention discloses a cationic polymer emulsifying wax which is obtained by copolymerizing cationic monomers. The invention discloses a preparation method of cationic polymer emulsifying wax, which comprises the following steps: in an absolute ethyl alcohol solvent, a cationic monomer is subjected to free radical polymerization reaction under the initiation action of an initiator to obtain the cationic polymer surfactant. The cationic polymer surfactant can be used as emulsifying wax to prepare wax emulsion with uniformly distributed particle size. The surface tension range of the cationic polymer surfactant prepared by the invention is 42 mN/m-58 mN/m, and the invention also discloses a particle size distribution diagram of the cationic polymer emulsifying wax.
Description
Technical Field
The invention belongs to the technical field of wax emulsion, and particularly relates to cationic polymer emulsifying wax and a preparation method thereof.
Background
The wax emulsion is an oil-water multiphase dispersion system, and can be dispersed into a stable emulsion in water under the action of a surfactant. In the manufacturing process, water is used as an organic solvent, so that the harm to the environment is reduced, the cost of the wax product is greatly reduced, and the application field of the wax product is expanded. The wax emulsion has the excellent performances of no toxicity, uniform film formation, abrasion resistance, scratch resistance and the like, and is widely applied to the fields of leather polishing oil, water-based paint, artificial plates, metal protection and the like.
The wax emulsion is a thermodynamically unstable system, and a proper surfactant and a preparation process are selected to prepare a wax emulsion product with stable performance. Emulsifiers, i.e., surfactants, are key factors in the preparation of stable wax emulsions. The lipophilic and hydrophilic amphiphilic chain segment of the high molecular surfactant can be anchored on a phase interface, and meanwhile, a certain interface film is formed at the phase interface, so that the emulsion wax particles are protected to a certain extent, and the dispersed particles are prevented from being coalesced, thereby forming a stable emulsion.
The cationic emulsifying wax has positive charges on the particle surfaces, so that the cationic emulsifying wax is easy to adsorb on the solid surfaces with negative charges, the film forming property of the solid surfaces is improved, and the coverage of the solid surfaces is increased. However, cationic emulsifying waxes are prone to delamination and few successful cationic emulsifying wax products. The stability of the cationic emulsifying wax can be improved by a mode of preparing the cationic high molecular surfactant.
Disclosure of Invention
The invention aims to provide a cationic polymer emulsifying wax and a preparation method thereof, wherein the cationic polymer emulsifying wax is obtained by copolymerizing cationic monomers, and the cationic polymer surfactant has excellent surface activity and better particle size distribution when used as an emulsifier.
The technical scheme adopted by the invention is as follows:
the cationic polymer emulsifying wax is characterized in that:
the composite material comprises the following components in percentage by mass:
5 to 10 percent of cationic polymer surfactant;
15% -45% of wax;
the balance being water.
The cationic polymer surfactant comprises the following components in percentage by mass:
20 to 50 percent of cationic monomer;
the balance of absolute ethyl alcohol.
The structural formula of the cationic monomer is as follows:
wherein R is1Is C1-C20Linear or branched alkyl of (a); r2Is C1-C20Linear or branched alkyl.
The wax is one or a mixture of two of beeswax, carnauba wax and paraffin wax in any proportion.
The preparation method of the cationic polymer emulsifying wax is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparation of cationic polymer surfactant:
taking 20-50% of cationic monomer and the balance of absolute ethyl alcohol by mass percentage; dissolving a cationic monomer in absolute ethyl alcohol, and then adding an oil-soluble initiator accounting for 0.5-2% of the mass of the cationic monomer to obtain a monomer mixed solution;
pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 70-85 ℃, carrying out reflux reaction for 4-8 h, cooling the obtained product to room temperature, and carrying out reduced pressure distillation and concentration to remove the solvent to obtain a transparent cationic polymer surfactant;
step two: preparation of cationic polymer emulsifying wax:
and (2) taking 15-45% of wax and 5-10% of the cationic polymer surfactant obtained in the step one by mass percent, sequentially adding the wax and the cationic polymer surfactant into a three-neck flask, heating to 60-90 ℃, after fully dissolving and uniformly mixing, slowly adding water under the stirring condition of 1000rpm, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
The oil-soluble initiator in the first step is azobisisobutyronitrile.
And the temperature of the water in the second step is 60-90 ℃.
The invention has the beneficial effects that:
1) the invention takes absolute ethyl alcohol as solvent, adopts a free radical copolymerization method to prepare the cationic polymer surfactant, has mature synthesis method, and has controllable and adjustable structure of the synthesized polymer surfactant.
2) The surface tension range of the macromolecular surfactant is 42 mN/m-58 mN/m, and the macromolecular surfactant can be used as an emulsified oily substance.
3) When the polymer surfactant is used for emulsifying wax, the cationic surfactant increases the aggregation resistance among particles, improves the stability of the wax emulsion, and the prepared wax emulsion has narrow particle size distribution range, single peak distribution and small particle size, and is nano-scale.
4) The wax emulsion takes water as a main solvent, is harmless to the environment and human body, is easy to be compounded with aqueous solution or emulsion of other substances for use, can integrally improve the hardness, scratch resistance, gloss durability and the like of a product coating film, and can be widely applied to the fields of water-based paint, paper sizing, leather processing and the like.
Drawings
FIG. 1 is a graph showing the effect of particle size of a cationic polymer emulsifying wax.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
The invention provides a cationic polymer emulsifying wax which comprises the following components in percentage by mass:
5 to 10 percent of cationic polymer surfactant;
15% -45% of wax;
the balance being water.
The cationic polymer surfactant comprises the following components in percentage by mass:
20 to 50 percent of cationic monomer;
the balance of absolute ethyl alcohol.
The structural formula of the cationic monomer is as follows:
wherein R is1Is C1-C20Linear or branched alkyl of (a); r2Is C1-C20Linear or branched alkyl.
The wax is one or a mixture of two of beeswax, carnauba wax and paraffin wax in any proportion.
The preparation method of the cationic polymer emulsifying wax comprises the following steps:
the method comprises the following steps: preparation of cationic polymer surfactant:
taking 20-50% of cationic monomer and the balance of absolute ethyl alcohol by mass percentage; dissolving a cationic monomer in absolute ethyl alcohol, and then adding an oil-soluble initiator accounting for 0.5-2% of the mass of the cationic monomer to obtain a monomer mixed solution;
pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 70-85 ℃, carrying out reflux reaction for 4-8 h, cooling the obtained product to room temperature, and carrying out reduced pressure distillation and concentration to remove the solvent to obtain a transparent cationic polymer surfactant;
step two: preparation of cationic polymer emulsifying wax:
and (2) taking 15-45% of wax and 5-10% of the cationic polymer surfactant obtained in the step one by mass percent, sequentially adding the wax and the cationic polymer surfactant into a three-neck flask, heating to 60-90 ℃, after fully dissolving and uniformly mixing, slowly adding water under the stirring condition of 1000rpm, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
The oil-soluble initiator in the first step is azobisisobutyronitrile.
And the temperature of the water in the second step is 60-90 ℃.
Example 1:
dissolving 20 mass percent of cationic monomer in absolute ethyl alcohol, adding an oil-soluble initiator azodiisobutyronitrile accounting for 0.5 mass percent of the total mass of the monomers, pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 70 ℃, carrying out reflux reaction for 4 hours, cooling the obtained product to room temperature, carrying out reduced pressure distillation and concentration to remove the solvent, and obtaining the transparent cationic polymer surfactant product. The surface tension was 42mN/m (mass concentration: 0.2%). Sequentially adding 15% of paraffin and 5% of cationic polymer surfactant into a three-neck flask, heating to 65 ℃, after the paraffin and the cationic polymer surfactant are fully dissolved and uniformly mixed, slowly adding 65 ℃ hot water under the stirring condition of 1000rpm, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
Wherein, the structural formula of the cationic monomer is as follows:
example 2:
dissolving 35% of cationic monomer by mass in absolute ethyl alcohol, adding an oil-soluble initiator azodiisobutyronitrile accounting for 1% of the total mass of the monomer, pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 75 ℃, carrying out reflux reaction for 4 hours, cooling the obtained product to room temperature, carrying out reduced pressure distillation and concentration, and removing the solvent to obtain the transparent cationic polymer surfactant product. The surface tension was 49mN/m (mass concentration: 0.2%). Sequentially adding 20% of palm wax and 7% of cationic polymer surfactant into a three-neck flask, heating to 90 ℃, slowly adding 90 ℃ hot water under the stirring condition of 1000rpm after the two are fully dissolved and uniformly mixed, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
Wherein, the structural formula of the cationic monomer is as follows:
example 3:
dissolving 40 mass percent of cationic monomer in absolute ethyl alcohol, adding an oil-soluble initiator azodiisobutyronitrile accounting for 1.5 mass percent of the total mass of the monomers, pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 80 ℃, carrying out reflux reaction for 4 hours, cooling the obtained product to room temperature, carrying out reduced pressure distillation and concentration, and removing the solvent to obtain the transparent cationic polymer surfactant product. The surface tension was 52mN/m (mass concentration: 0.2%). Sequentially adding 35% of beeswax and 8% of cationic polymer surfactant into a three-neck flask, heating to 70 ℃, after the beeswax and the cationic polymer surfactant are fully dissolved and uniformly mixed, slowly adding hot water with the temperature of 70 ℃ under the stirring condition of 1000rpm, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
Wherein, the structural formula of the cationic monomer is as follows:
example 4:
dissolving 50 mass percent of cationic monomer in absolute ethyl alcohol, adding an oil-soluble initiator azobisisobutyronitrile accounting for 2 mass percent of the total mass of the monomer, pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 85 ℃, carrying out reflux reaction for 4 hours, cooling the obtained product to room temperature, carrying out reduced pressure distillation and concentration, and removing the solvent to obtain the transparent cationic polymer surfactant product. The surface tension was 58mN/m (mass concentration: 0.2%). Adding 45% paraffin and 10% cationic polymer surfactant into a three-neck flask in sequence, heating to 70 deg.C, slowly adding 70 deg.C hot water under stirring at 1000rpm after the two are dissolved sufficiently, and stirring for 30min to obtain cationic polymer emulsifying wax.
Wherein, the structural formula of the cationic monomer is as follows:
example 5:
dissolving 30 mass percent of cationic monomer in absolute ethyl alcohol, adding an oil-soluble initiator azodiisobutyronitrile accounting for 1.5 mass percent of the total mass of the monomers, pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 80 ℃, carrying out reflux reaction for 4 hours, cooling the obtained product to room temperature, carrying out reduced pressure distillation and concentration to remove the solvent, and obtaining the transparent cationic polymer surfactant product. The surface tension was 50mN/m (mass concentration: 0.2%). Sequentially adding 32% of beeswax and 9% of cationic polymer surfactant into a three-neck flask, heating to 75 ℃, slowly adding 75 ℃ hot water under the stirring condition of 1000rpm after the beeswax and the cationic polymer surfactant are fully dissolved and uniformly mixed, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
Wherein, the structural formula of the cationic monomer is as follows:
and (3) testing the performance of the prepared high molecular surfactant:
surface tension test: the surface tension of the high molecular surfactant is measured by a hanging ring method at 25 ℃ by adopting a Chengdu-Jian XJZ-200 type surface tension meter. A series of different concentrations of the polymeric surfactant emulsion were placed in a beaker. The instrument was first calibrated with redistilled water (γ: 72.1 ± 0.01mN/m) and absolute ethanol (γ: 22.3 ± 0.01 mN/m). In order to improve the test precision of the surface tension, the surface tension of the high molecular surfactant is determined by adopting a method of averaging three experiments.
And (3) particle size testing:
the particle size (Dz) and the distribution (expressed as polydispersity PDI) of the wax emulsion were determined using a laser scattering particle sizer model Nano ZS, Malvern Zetasizer, uk, at a test temperature of 25 ℃. The wax emulsion was diluted to 0.2% mass concentration with deionized water, and subjected to ultrasonic dispersion treatment for 30min, followed by testing.
Referring to the particle size effect diagram of the cationic polymer emulsifying wax in fig. 1, it can be seen that the particle size of the cationic polymer emulsifying wax emulsion prepared by the present invention shows unimodal distribution, narrow particle size distribution range, 0.095 polydispersion coefficient and 57.75nm particle size, which indicates that the cationic polymer surfactant prepared by the free radical copolymerization method can be used for emulsifying wax, and the prepared wax emulsion has small particle size and high stability.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.
Claims (4)
1. The cationic polymer emulsifying wax is characterized by comprising, by mass, 5-10% of a cationic polymer surfactant, 15-45% of wax and the balance water;
the preparation method of the cationic polymer emulsifying wax comprises the following steps:
1) preparation of cationic polymer surfactant: taking 20-50% of cationic monomer and the balance of absolute ethyl alcohol by mass percentage; dissolving a cationic monomer in absolute ethyl alcohol, and then adding an oil-soluble initiator accounting for 0.5-2% of the mass of the cationic monomer to obtain a monomer mixed solution;
the structural formula of the cationic monomer is as follows:
wherein R is1Is C1-C20Linear or branched alkyl of (a); r2Is C1-C20Linear or branched alkyl of (a);
pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 70-85 ℃, carrying out reflux reaction for 4-8 h, cooling the obtained product to room temperature, and carrying out reduced pressure distillation and concentration to remove the solvent to obtain a transparent cationic polymer surfactant;
2) preparation of cationic polymer emulsifying wax: taking 15-45% of wax and 5-10% of the cationic polymer surfactant obtained in the step 1), sequentially adding the wax and the cationic polymer surfactant into a three-neck flask, heating to 60-90 ℃, after fully dissolving and uniformly mixing, slowly adding water under the stirring condition of 1000rpm, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax;
the wax is one or a mixture of two of beeswax, carnauba wax and paraffin wax in any proportion.
2. A method for producing the cationic polymer emulsifying wax according to claim 1, comprising:
1) preparation of cationic polymer surfactant: taking 20-50% of cationic monomer and the balance of absolute ethyl alcohol by mass percentage; dissolving a cationic monomer in absolute ethyl alcohol, and then adding an oil-soluble initiator accounting for 0.5-2% of the mass of the cationic monomer to obtain a monomer mixed solution;
pouring the monomer mixed solution into a four-neck flask provided with a stirrer and a thermometer, introducing nitrogen, stirring, heating, controlling the reaction temperature to be 70-85 ℃, carrying out reflux reaction for 4-8 h, cooling the obtained product to room temperature, and carrying out reduced pressure distillation and concentration to remove the solvent to obtain a transparent cationic polymer surfactant;
2) preparation of cationic polymer emulsifying wax: taking 15-45% of wax and 5-10% of the cationic polymer surfactant obtained in the step 1), sequentially adding the wax and the cationic polymer surfactant into a three-neck flask, heating to 60-90 ℃, after fully dissolving and uniformly mixing, slowly adding water under the stirring condition of 1000rpm, and continuously stirring for 30min to obtain the cationic polymer emulsifying wax.
3. The method of claim 2, wherein the oil-soluble initiator in step 1) is azobisisobutyronitrile.
4. The method for preparing the cationic polymer emulsifying wax of claim 2, wherein the temperature of the added water in the step 2) is 60 to 90 ℃.
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