CN110577653A - Emulsion nano composite emulsion based on electrostatic self-assembly and preparation method thereof - Google Patents
Emulsion nano composite emulsion based on electrostatic self-assembly and preparation method thereof Download PDFInfo
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- CN110577653A CN110577653A CN201910850358.6A CN201910850358A CN110577653A CN 110577653 A CN110577653 A CN 110577653A CN 201910850358 A CN201910850358 A CN 201910850358A CN 110577653 A CN110577653 A CN 110577653A
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- 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
- 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
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C3/00—Tanning; Compositions for tanning
- C14C3/02—Chemical tanning
- C14C3/08—Chemical tanning by organic agents
- C14C3/22—Chemical tanning by organic agents using polymerisation products
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- 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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
Abstract
The invention discloses an emulsion nano composite emulsion based on electrostatic self-assembly and a preparation method thereof, which have the advantages of low cost, environment-friendly preparation method and good product stability and can be used for leather retanning. The technical scheme of the invention is as follows: a preparation method of an emulsion nano composite emulsion based on electrostatic self-assembly is characterized in that waterborne polyurethane is prepared by adopting a one-pot method, hydrotalcite is dispersed in water and added in a polyurethane emulsification stage, so that the hydrotalcite is uniformly dispersed in a polyurethane matrix, and the hydrotalcite and the polyurethane are assembled by utilizing the positive point property of the hydrotalcite and the electronegativity of the polyurethane, so that the emulsion nano composite emulsion based on electrostatic self-assembly is prepared. According to the invention, the hydrotalcite is used as a nano material to modify the waterborne polyurethane, the material is easy to prepare and low in cost, the preparation method is simple and environment-friendly, and the product stability is good; the prepared hydrotalcite-coated polyurethane nano composite emulsion can be used for leather retanning, can improve the dye absorption rate in the leather making process, reduces the wastewater pollution, and endows the finished leather with certain flame retardant property.
Description
Technical Field
The invention belongs to the field of polymer nano composite materials, and particularly relates to an emulsion nano composite emulsion based on electrostatic self-assembly and a preparation method thereof.
Background
The water-based polyurethane is a retanning agent with excellent comprehensive performance, and because a large amount of carbamate groups similar to the chain structure (amido bonds) of the collagen peptide of the natural leather are contained in the molecular chain, the water-based polyurethane can not only keep the natural hand feeling of the leather when being used for leather retanning, but also endow the leather with excellent flexibility and dyeing property. The traditional polyurethane retanning agent has the defects of poor thermal stability, poor retanning performance, single functionality and the like. Therefore, the retanning performance of polyurethane can be improved and the functionality can be endowed by properly modifying the polyurethane retanning agent.
The organic-inorganic nano composite material combines the characteristics of organic and inorganic materials, such as thermal stability, solubility, processability and the like, and is a new generation composite material with high performance and multiple functions. The water-based polyurethane matrix can be reinforced and modified by adopting inorganic nano materials such as hydrotalcite, graphene, silicon dioxide and the like, so that the defects of the matrix material can be effectively overcome, the thermal stability of the matrix material can be improved, and the composite material can be endowed with new performances such as electric conductivity, thermal conductivity, heat insulation, flame retardance, adsorbability and the like.
Hydrotalcite is a layered metal hydroxide, and has the characteristics of enhancing the thermal stability of a substrate and endowing the substrate with adsorbability and flame retardance. The hydrotalcite has weak positive properties, and is introduced into the anionic polyurethane, and because the hydrotalcite and the anionic polyurethane have different charges, self-assembly behavior can be generated based on electrostatic acting force, so that the hydrotalcite-coated polyurethane nano composite emulsion is formed. The nano composite material is used for leather retanning, and can play a role in retanning and filling leather; meanwhile, the adsorption and the flame retardance of the hydrotalcite are utilized to improve the dye adsorption rate in the retanning process, reduce the pollution of waste water and endow the finished leather with certain flame retardant functionality.
disclosure of Invention
The invention aims to provide the electrostatic self-assembly based emulsion nano composite emulsion and the preparation method thereof, which utilize the characteristic that the hydrotalcite and the polyurethane have different electrical properties to enable the hydrotalcite and the polyurethane to be self-assembled, have the advantages of easy preparation of materials, low cost, simple and environment-friendly preparation method and good product stability, and can be used for leather retanning.
In order to achieve the aim, the invention provides a preparation method of an emulsion nano composite emulsion based on electrostatic self-assembly,
The method comprises the steps of preparing waterborne polyurethane by adopting a one-pot method, dispersing hydrotalcite in water, adding the hydrotalcite in a polyurethane emulsification stage to uniformly disperse the hydrotalcite in a polyurethane matrix, and assembling the hydrotalcite and the polyurethane by utilizing the positive point property of the hydrotalcite and the electronegativity of the polyurethane to prepare the emulsion nano composite emulsion based on electrostatic self-assembly.
The preparation method of the emulsion nano composite emulsion based on electrostatic self-assembly comprises the following specific steps:
step one, preparing a hydrotalcite nano-sheet layer:
Firstly, 0.03 ~ 0.3.3 mol of nitrate A, 0.03 ~ 0.2.2 mol of nitrate B and 0.001 ~ 0.05.05 mol of anhydrous sodium carbonate are weighed and dissolved in 100 ~ 300mL of deionized water, the pH value is adjusted to 6 ~ 13, the mixture is stirred and reacted for 1 ~ 3h at the temperature of 70 ~ 100 ℃, then the mixture is subjected to heat preservation and crystallization for 10 ~ 18h, and after the reaction is finished, the hydrotalcite nano material is obtained through filtering, washing, drying and grinding;
nitrate A being Mg (NO)3)2、Ni (NO3)2、Zn (NO3)2、Ca (NO3)2、Cu (NO3)2、Cd (NO3)2Or Co (NO)3)2；
Nitrate B being Al (NO)3)3、Ga (NO3)3、In (NO3)3Or Cr (NO)3)3；
Step two, preparing the hydrotalcite-coated polyurethane nano composite emulsion:
firstly, weighing 10 ~ 20g of polyol, heating to 100 ~ 120 ℃, vacuumizing and stirring for 1 ~ 2h until complete dehydration, then reducing the temperature of the system to 50 ~ 70 ℃, adding 1 ~ 3g of 2, 2-dihydroxybutyric acid, dissolving and stirring uniformly, continuing to increase the temperature to 70 ~ 90 ℃, dropwise adding 3 ~ 9g of diisocyanate, carrying out heat preservation and polymerization for 1 ~ 5h at a stirring speed of 200 ~ 400r/min, reducing the temperature to 40 ℃ after the reaction is finished, adding 0.5-2mL of triethylamine for neutralization, adding the water dispersion of hydrotalcite in the emulsification stage of waterborne polyurethane, stirring vigorously for 1h at a rotation speed of 800-.
In the second step, the preparation method of the hydrotalcite aqueous dispersion comprises the step of dispersing hydrotalcite with the mass fraction of 0wt% -10wt% in 40-100mL of water.
In the second step, the time of the emulsification reaction is 0.5 ~ 2h, the stirring speed during the emulsification reaction is 800 ~ 1400r/min, and the diisocyanate is toluene diisocyanate, diphenylmethane diisocyanate or isophorone diisocyanate.
In the first step, NaOH aqueous solution with the pH value of 1 ~ 3mol/L is used for adjusting the pH value, and the nitrate A is Mg (NO)3)2nitrate B is Al (NO)3)3。
the hydrotalcite-coated polyurethane nano composite emulsion is prepared by the preparation method.
compared with the prior art, the invention has the beneficial effects that:
1. According to the invention, the hydrotalcite is used as a nano material to modify the waterborne polyurethane, and the hydrotalcite and the polyurethane have different electrical properties, so that the hydrotalcite and the polyurethane are self-assembled to obtain the hydrotalcite-coated polyurethane nano emulsion.
2. The hydrotalcite-coated polyurethane nano composite emulsion provided by the invention can be used for leather retanning, can improve the dye absorption rate in the leather making process and reduce the wastewater pollution, and can endow the finished leather with certain flame retardant property.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention include, but are not limited to, the scope shown in the following examples.
According to the invention, the polyurethane is modified by using hydrotalcite, and the hydrotalcite nanosheet layer is coated on the outer layer of the polyurethane to obtain the WPU @ LDH nano composite emulsion which has good organic-inorganic phase compatibility and stable emulsion.
The preparation method of the hydrotalcite-coated polyurethane nano composite emulsion comprises the following specific preparation steps:
The method comprises the following steps: preparing a hydrotalcite nano-sheet layer;
firstly, 0.03 ~ 0.3.3 mol of nitrate A, 0.03 ~ 0.2.2 mol of nitrate B and 0.001 ~ 0.05.05 mol of anhydrous sodium carbonate are weighed and dissolved in 100 ~ 300mL of deionized water, 1 ~ 3mol/L of NaOH aqueous solution is used for adjusting the pH value to 6 ~ 13, the mixture is stirred and reacted for 1 ~ 3h at the temperature of 70 ~ 100 ℃, then the mixture is subjected to heat preservation and crystallization for 10 ~ 18h, and after the reaction is finished, the hydrotalcite nano material is obtained through filtration, washing, drying and grinding;
Nitrate A being Mg (NO)3)2、Ni (NO3)2、Zn (NO3)2、Ca (NO3)2、Cu (NO3)2、Cd (NO3)2Or Co (NO)3)2；
nitrate B being Al (NO)3)3、Ga (NO3)3、In (NO3)3or Cr (NO)3)3；
step two: preparing hydrotalcite coated polyurethane nano composite emulsion;
firstly, weighing 10 ~ 20g of polyol, heating to 100 ~ 120 ℃, vacuumizing and stirring for 1 ~ 2h until complete dehydration, then, reducing the temperature of the system to 50 ~ 70 ℃, adding 1 ~ 3g of 2, 2-dihydroxybutyric acid, dissolving and stirring uniformly, continuing to increase the temperature to 70 ~ 90 ℃, dropwise adding 3 ~ 9g of diisocyanate, carrying out thermal polymerization for 1 ~ 5h, stirring at the speed of 200 ~ 400r/min, after the reaction is finished, reducing the temperature to 40 ℃, adding 0.5-2mL of triethylamine for neutralization, dispersing 0-10 wt% of hydrotalcite in 40-100mL of water to prepare an aqueous dispersion of the hydrotalcite, adding the aqueous dispersion of the hydrotalcite in the emulsification stage of the aqueous polyurethane, violently stirring for 1h, rotating at the speed of 800-.
In the first step, the nitrate A is Mg (NO)3)2Nitrate B is Al (NO)3)3。
in the second step, the diisocyanate is toluene diisocyanate, diphenylmethane diisocyanate or isophorone diisocyanate.
Example 1
the method comprises the following steps: preparing a hydrotalcite nano-sheet layer;
firstly, weighing 0.2mol of magnesium nitrate, 0.1mol of aluminum nitrate and 0.04mol of anhydrous sodium carbonate, dissolving in 120mL of deionized water, adjusting the pH to 10 by using 1mol/L NaOH aqueous solution, stirring and reacting at the temperature of 80 ℃ for 1h, then carrying out heat preservation and crystallization for 12h, and filtering, washing, drying and grinding after the reaction is finished to obtain the magnesium-aluminum hydrotalcite nano material;
step two: preparing hydrotalcite coated polyurethane (WPU @ LDH) nano composite emulsion;
Firstly, weighing 20g of polyethylene glycol, heating to 120 ℃, vacuumizing and stirring for 2 hours until the mixture is completely dehydrated; then, the temperature of the system is reduced to 60 ℃, 1.25g of 2, 2-dihydroxybutyric acid is added, the mixture is dissolved and stirred evenly, the temperature is increased to 80 ℃, 5.07g of isophorone diisocyanate is added dropwise, the mixture is polymerized for 3 hours in a heat preservation way, and the stirring speed is 300 r/min. After the reaction, the temperature was reduced to 40 ℃ and 1.18mL of triethylamine was added for neutralization. An aqueous hydrotalcite dispersion was prepared by dispersing 2wt% hydrotalcite in 64mL of water. Adding hydrotalcite aqueous dispersion liquid at the emulsification stage of waterborne polyurethane, stirring vigorously for 1h at the rotation speed of 1000r/min, and standing to obtain hydrotalcite-coated polyurethane (WPU @ LDH) nano composite emulsion.
Example 2
The method comprises the following steps: preparing a hydrotalcite nano-sheet layer;
Firstly, weighing 0.3mol of zinc nitrate, 0.15mol of aluminum nitrate and 0.05mol of anhydrous sodium carbonate, dissolving in 100mL of deionized water, adjusting the pH to 10 by using 1mol/L NaOH aqueous solution, stirring and reacting at the temperature of 85 ℃ for 5 hours, then carrying out heat preservation and crystallization for 10 hours, and filtering, washing, drying and grinding after the reaction is finished to obtain the zinc-aluminum hydrotalcite nano material;
Step two: preparing hydrotalcite coated polyurethane (WPU @ LDH) nano composite emulsion;
firstly, weighing 15g of polyethylene glycol, heating to 120 ℃, vacuumizing and stirring for 2 hours until the mixture is completely dehydrated; then, the temperature of the system is reduced to 60 ℃, 0.94g of 2, 2-dihydroxybutyric acid is added, the mixture is dissolved and stirred evenly, the temperature is increased to 80 ℃, 3.8g of isophorone diisocyanate is added dropwise, the mixture is polymerized for 3 hours in a heat preservation way, and the stirring speed is 300 r/min. After the reaction, the temperature was reduced to 40 ℃ and 0.88mL of triethylamine was added for neutralization. An aqueous dispersion of hydrotalcite was prepared by dispersing hydrotalcite 6wt% in 50mL of water. Adding hydrotalcite aqueous dispersion liquid at the emulsification stage of waterborne polyurethane, stirring vigorously for 1h at the rotation speed of 1000r/min, and standing to obtain hydrotalcite-coated polyurethane (WPU @ LDH) nano composite emulsion.
Example 3
The method comprises the following steps: preparing a hydrotalcite nano-sheet layer;
firstly, weighing 0.3mol of magnesium nitrate, 0.15mol of aluminum ferric nitrate and 0.05mol of anhydrous sodium carbonate, dissolving in 100mL of deionized water, adjusting the pH to 9 by using 1mol/L NaOH aqueous solution, stirring and reacting at the temperature of 85 ℃ for 5 hours, then carrying out heat preservation and crystallization for 10 hours, and filtering, washing, drying and grinding after the reaction is finished to obtain the magnesium-iron hydrotalcite nano material;
step two: preparing hydrotalcite coated polyurethane (WPU @ LDH) nano composite emulsion;
firstly, weighing 15g of polyethylene glycol, heating to 120 ℃, vacuumizing and stirring for 2 hours until the mixture is completely dehydrated; then, the temperature of the system is reduced to 60 ℃, 0.94g of 2, 2-dihydroxybutyric acid is added, the mixture is dissolved and stirred evenly, the temperature is increased to 80 ℃, 3.8g of isophorone diisocyanate is added dropwise, the mixture is polymerized for 3 hours in a heat preservation way, and the stirring speed is 300 r/min. After the reaction, the temperature was reduced to 40 ℃ and 0.88mL of triethylamine was added for neutralization. An aqueous dispersion of hydrotalcite was prepared by dispersing 4wt% of hydrotalcite in 50mL of water. Adding hydrotalcite aqueous dispersion liquid at the emulsification stage of waterborne polyurethane, stirring vigorously for 1h at the rotation speed of 1100r/min, and standing to obtain hydrotalcite-coated polyurethane (WPU @ LDH) nano composite emulsion.
Example 4
the method comprises the following steps: preparing a hydrotalcite nano-sheet layer;
Firstly, weighing 0.2mol of copper nitrate, 0.1mol of aluminum nitrate and 0.04mol of anhydrous sodium carbonate, dissolving in 900mL of deionized water, adjusting the pH to 9 by using 1mol/L NaOH aqueous solution, stirring and reacting at the temperature of 80 ℃ for 2 hours, then carrying out heat preservation and crystallization for 10 hours, and filtering, washing, drying and grinding after the reaction is finished to obtain the copper-aluminum hydrotalcite nano material;
step two: preparing hydrotalcite coated polyurethane (WPU @ LDH) nano composite emulsion;
Firstly, weighing 20g of polyethylene glycol, heating to 120 ℃, vacuumizing and stirring for 2 hours until the mixture is completely dehydrated; then, the temperature of the system is reduced to 60 ℃, 1.25g of 2, 2-dihydroxybutyric acid is added, the mixture is dissolved and stirred evenly, the temperature is increased to 80 ℃, 5.07g of isophorone diisocyanate is added dropwise, the mixture is polymerized for 3 hours in a heat preservation way, and the stirring speed is 300 r/min. After the reaction, the temperature was reduced to 40 ℃ and 1.18mL of triethylamine was added for neutralization. An aqueous dispersion of hydrotalcite was prepared by dispersing 10wt% of hydrotalcite in 65mL of water. Adding hydrotalcite aqueous dispersion liquid at the emulsification stage of waterborne polyurethane, stirring vigorously for 2h at the rotation speed of 1200r/min, and standing to obtain hydrotalcite-coated polyurethane (WPU @ LDH) nano composite emulsion.
In order to test the retanning performance of the hydrotalcite coated polyurethane (WPU @ LDH) nano composite emulsion prepared by the invention, the inventor conducts retanning application experiments on the hydrotalcite coated polyurethane (WPU @ LDH) nano composite emulsion, and obtains the influence of nano composite materials with different hydrotalcite dosages on retanning through analysis. The blank polyurethane solution has poor dispersibility, the microstructure is 500 +/-100 nm of irregular polymer, hydrotalcite is added, and the hydrotalcite-coated polyurethane microspheres with the particle size of 200 +/-20 nm are formed through electrostatic self-assembly. The composite material is used for retanning goat blue wet leather, and compared with empty-packed polyurethane, when the using amount of the magnesium-aluminum hydrotalcite is 2wt%, the dye absorption rate is increased from 94.8% to 98.0%, and the biological oxygen Consumption (COD) of waste liquid is increasedCr) The softness, mechanical property, thickening rate and the like of the finished leather are all improved when the concentration is reduced from 4393mg/L to 3600 mg/L. And the addition of the hydrotalcite endows the finished leather with certain flame retardant property, when the using amount of the magnesium-aluminum LDH is 8%, the flame retardant property of the finished leather is optimal, and the open flame time, the total heat release amount, the heat release rate and the like are obviously reduced.
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 (6)
1. A preparation method of an emulsion nano composite emulsion based on electrostatic self-assembly is characterized by comprising the following steps:
The method comprises the steps of preparing waterborne polyurethane by adopting a one-pot method, dispersing hydrotalcite in water, adding the hydrotalcite in a polyurethane emulsification stage to uniformly disperse the hydrotalcite in a polyurethane matrix, and assembling the hydrotalcite and the polyurethane by utilizing the positive point property of the hydrotalcite and the electronegativity of the polyurethane to prepare the emulsion nano composite emulsion based on electrostatic self-assembly.
2. The method for preparing the emulsion nanocomposite emulsion based on electrostatic self-assembly according to claim 1, wherein the method comprises the following steps:
the method comprises the following specific steps:
step one, preparing a hydrotalcite nano-sheet layer:
Firstly, 0.03 ~ 0.3.3 mol of nitrate A, 0.03 ~ 0.2.2 mol of nitrate B and 0.001 ~ 0.05.05 mol of anhydrous sodium carbonate are weighed and dissolved in 100 ~ 300mL of deionized water, the pH value is adjusted to 6 ~ 13, the mixture is stirred and reacted for 1 ~ 3h at the temperature of 70 ~ 100 ℃, then the mixture is subjected to heat preservation and crystallization for 10 ~ 18h, and after the reaction is finished, the hydrotalcite nano material is obtained through filtering, washing, drying and grinding;
Nitrate A being Mg (NO)3)2、Ni (NO3)2、Zn (NO3)2、Ca (NO3)2、Cu (NO3)2、Cd (NO3)2Or Co (NO)3)2；
Nitrate B being Al (NO)3)3、Ga (NO3)3、In (NO3)3Or Cr (NO)3)3；
step two, preparing the hydrotalcite-coated polyurethane nano composite emulsion:
firstly, weighing 10 ~ 20g of polyol, heating to 100 ~ 120 ℃, vacuumizing and stirring for 1 ~ 2h until complete dehydration, then reducing the temperature of the system to 50 ~ 70 ℃, adding 1 ~ 3g of 2, 2-dihydroxybutyric acid, dissolving and stirring uniformly, continuing to increase the temperature to 70 ~ 90 ℃, dropwise adding 3 ~ 9g of diisocyanate, carrying out heat preservation and polymerization for 1 ~ 5h at a stirring speed of 200 ~ 400r/min, reducing the temperature to 40 ℃ after the reaction is finished, adding 0.5-2mL of triethylamine for neutralization, adding the water dispersion of hydrotalcite in the emulsification stage of waterborne polyurethane, stirring vigorously for 1h at a rotation speed of 800-.
3. The method for preparing the emulsion nanocomposite emulsion based on electrostatic self-assembly according to claim 2, wherein the method comprises the following steps:
In the first step, a 1 ~ 3mol/L NaOH aqueous solution is used for adjusting the pH.
4. The method for preparing the emulsion nanocomposite emulsion based on electrostatic self-assembly according to claim 3, wherein the method comprises the following steps:
In the second step, the preparation method of the hydrotalcite aqueous dispersion comprises the step of dispersing hydrotalcite with the mass fraction of 0-10% in 40-100mL of water.
5. The method for preparing the emulsion nanocomposite emulsion based on electrostatic self-assembly according to claim 4, wherein the method comprises the following steps:
In the second step, the time of the emulsification reaction is 0.5 ~ 2h, the stirring speed during the emulsification reaction is 800 ~ 1400r/min, and the diisocyanate is toluene diisocyanate, diphenylmethane diisocyanate or isophorone diisocyanate.
6. a hydrotalcite coated polyurethane nanocomposite emulsion obtained by the process according to claims 1 to 5.
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| CN115093683A (en) * | 2022-06-08 | 2022-09-23 | 青岛普诺恩生物科技有限公司 | Modified degradable material with controllable degradation rate and preparation method thereof |
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