CN109866298B - Paraffin-based Pickering emulsion containing hybrid montmorillonite and preparation method thereof - Google Patents
Paraffin-based Pickering emulsion containing hybrid montmorillonite and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of wood waterproofing agents, in particular to paraffin-based Pickering emulsion containing hybrid montmorillonite and a preparation method thereof. In the emulsion prepared by the invention, the hybrid montmorillonite can be adsorbed on a paraffin/water interface to play a role in stabilizing the emulsion, and the dosage of the surfactant can be reduced on the premise of ensuring the stability of the emulsion, so that the negative influence of the surfactant on the waterproof effect of the emulsion is reduced.
Description
Technical Field
The invention relates to the field of wood waterproofing agents, in particular to a wood waterproofing agent containing hybrid montmorillonite.
Background
The main components of the cell wall of wood, cellulose, hemicellulose and lignin, contain a large number of hydroxyl groups, which cause the wood to have strong moisture (water) absorption, thereby causing large changes in wood size with changes in moisture content or external humidity, i.e., dimensional instability. Finally, the problems of dry shrinkage, wet swelling, deformation, cracking and the like of the wood are caused, and other properties of the wood are influenced to different degrees. Researchers have said that more than 90% of the defects in wood are related to moisture. Therefore, in wood treatment, waterproofing agents are often used to improve the waterproofing of wood.
Paraffin is an organic substance with strong hydrophobicity, and can be distributed in wood through physical adsorption to achieve the aim of water resistance. However, paraffin wax is insoluble in water and organic solvents, and is solid at ordinary temperature. The wood treatment needs to be carried out in a high-temperature melting state, the treatment process is complex, and the wood is not easy to be uniformly distributed in the treated wood, so that the waterproof effect of the wood is influenced. In order to overcome the defects of the paraffin waterproof agent, the emulsified paraffin waterproof agent is a better choice. Paraffin is used as a base material, and the paraffin is dispersed in a water phase in a form of small particles under the action of an emulsifier to form a homogeneous system of paraffin-based Pickering emulsion. By dipping the paraffin-based Pickering emulsion, the oil-water phase of the emulsion is separated during the drying process of the treated material, so that the paraffin is uniformly distributed in the treated material, and the hydrophobicity of the wood is improved. CN 103862538 discloses a paraffin-based water repellent based on natural surfactants, which is prepared by taking natural surfactants alkyl glycoside and span as emulsifiers and taking solid paraffin and water as raw materials. CN 104526805 discloses a method for preparing a non-ionic paraffin-based Pickering emulsion for wood modification, wherein a fatty alcohol ether polyoxyethylene type non-ionic surfactant is used as an emulsifier, a high-molecular film-forming agent is combined, an auxiliary emulsifier is not needed, a reverse phase emulsification method is adopted, water is added at one time to prepare the paraffin-based Pickering emulsion with small particle size and stability, and the obtained paraffin-based Pickering emulsion can be compounded with acidic liquid and alkaline liquid simultaneously, can be used for enhancing the waterproof and moisture-proof performance of solid wood and artificial boards, and can reduce the moisture absorption deformation of the solid wood and the artificial boards.
Although the traditional paraffin-based Pickering emulsion has a remarkable effect on improving the hydrophobicity of wood, more surfactant is required to be added in the preparation process of the emulsion in order to obtain a more ideal emulsification effect and a lower particle size. The modified wood water-proof agent has no positive effect on the improvement of the subsequent wood performance, even influences the improvement of the water-proof performance to a certain extent, and part of the surfactant with toxic action has certain pollution to the environment. In order to solve this problem, it is necessary to reduce the content of the surfactant in the paraffin water repellent as much as possible. In addition, the combustion heat value of the paraffin is 43MJ/kg, which is 3.6 times of that of wood, and the wood treated by the paraffin is easier to burn; the mechanical property of wood cannot be effectively improved by the traditional paraffin-based Pickering emulsion treatment, and the effect of one dose of the emulsion cannot be realized.
Disclosure of Invention
The invention aims to provide a paraffin-based Pickering emulsion containing hybrid montmorillonite, which is mainly improved in that the raw materials for preparing the emulsion contain the hybrid montmorillonite, and the hybrid montmorillonite is prepared by modifying the montmorillonite by silane, micromolecular alcohol and silicate ester.
The hybrid montmorillonite is added into the paraffin-based Pickering emulsion, and the hybridized montmorillonite solid particles are adsorbed on the surface of the paraffin in an adsorption mode.
Preferably, the preparation method of the hybrid montmorillonite comprises the steps of mixing silane, silicate ester, micromolecular alcohol, montmorillonite and water, fully and uniformly mixing, and removing water to obtain the hybrid montmorillonite.
As a preferable operation mode, the preparation method of the hybrid montmorillonite comprises the steps of mixing the materials and stirring at the speed of 2000-6000rpm for 2-10 hours at the temperature of 30-60 ℃.
Preferably, the mass ratio of the silane to the silicate to the small molecular alcohol to the montmorillonite is 1-2: 12-50: 12-50: 3 to 10.
Preferably, the silane is one or more of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltriethoxysilane or vinyltris (beta-methoxyethoxy) silane;
preferably, the silicate is one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate;
preferably, the montmorillonite is one or more of sodium montmorillonite, calcium montmorillonite or organic montmorillonite, and preferably sodium montmorillonite.
Preferably, the small molecular alcohol is one or more of methanol, ethanol, n-propanol or isopropanol, and ethanol is preferred.
Preferably, the raw materials for preparing the paraffin-based Pickering emulsion also comprise paraffin, a low HLB value nonionic surfactant and a high HLB value nonionic surfactant.
Preferably, the paraffin is liquid paraffin or solid paraffin, preferably 5# liquid paraffin or 50# solid paraffin;
preferably, the low HLB nonionic surfactant is one or more of propylene glycol monostearate, glyceryl monostearate, polyoxypropylene stearate, tetraethylene glycol monostearate, polyoxyethylene dioleate, sorbitan monooleate, or sorbitan monooleate, and preferably is sorbitan monooleate or sorbitan monooleate;
preferably, the high HLB nonionic surfactant is one or more of polyoxyethylene monostearate, polyoxyethylene cetyl alcohol, polyoxyethylene sorbitan monooleate, polyoxyethylene monolaurate or polyoxyethylene methyl glucoside hemioleate, and is preferably polyoxyethylene monostearate or polyoxyethylene monolaurate.
Preferably, when the using amount of water is 1L, the raw materials for preparing the paraffin-based Pickering emulsion comprise 10-80 g of hybrid montmorillonite, 200-700 g of paraffin, 10-50 g of low-HLB (hydrophile-lipophile balance) nonionic surfactant and 10-40 g of high-HLB nonionic surfactant.
Further preferably, when the using amount of water is 1L, the raw materials for preparing the paraffin-based Pickering emulsion comprise 50-70 g of hybrid montmorillonite, 400-500 g of paraffin, 20-32 g of low-HLB (hydrophile-lipophile balance) nonionic surfactant and 15-25 g of high-HLB nonionic surfactant;
preferably, in the above scheme, the low HLB nonionic surfactant is propylene glycol monostearate, sorbitan monooleate, or polyoxyethylene dioleate; the high HLB value nonionic surfactant is polyoxyethylene monostearate, polyoxyethylene methyl glucoside half oleate or polyoxyethylene sorbitan monooleate.
The invention also provides a preparation method of the paraffin-based Pickering emulsion, which comprises the following steps:
1) mixing the hybrid montmorillonite and paraffin at 70-95 ℃, adding a low HLB value nonionic surfactant and a high HLB value nonionic surfactant, and stirring at 5000-10000 rpm for 10-20min to prepare a primary emulsion;
2) and (3) homogenizing the primary emulsion for 1-2 times by a high-pressure homogenizer under the homogenizing pressure of 40-80 MPa to obtain the hybrid montmorillonite-stabilized paraffin-based Pickering emulsion wood.
The invention has the following beneficial effects:
1) according to the invention, the paraffin-based Pickering emulsion wood waterproofing agent is stabilized by using hybrid montmorillonite, so that the high-efficiency wood waterproofing agent with small particle size (less than 250nm) and high stability is obtained, and the wood waterproofing agent does not contain harmful chemical substances and is safe and environment-friendly.
2) In the waterproof agent prepared by the invention, the hybrid montmorillonite can be adsorbed on a paraffin/water interface to play a role in stabilizing the emulsion, and the dosage of the surfactant can be reduced on the premise of ensuring the stability of the emulsion, so that the negative influence of the surfactant on the waterproof effect of the emulsion is reduced.
3) Because the hybrid montmorillonite has thermal stability and rigidity, the wood is treated by the wood waterproofing agent of the paraffin-based Pickering emulsion stabilized by the hybrid montmorillonite, the flame retardant property and the mechanical property of the wood can be obviously improved, and the effect of one agent of multiple effects is realized. The waterproof agent can be applied to the fields of water proofing and moisture proofing of artificial boards and the like.
Drawings
FIG. 1 TEM-EDX results, FIG. 1 shows that a is comparative example 2, and FIGS. 1b and 1c are the results of example 2.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
This example relates to a paraffin-based Pickering emulsion containing hybrid montmorillonite.
The hybrid montmorillonite is prepared by the following method:
9g of gamma-aminopropyltrimethoxysilane, 150g of methyl orthosilicate, 150g of methanol and 40g of sodium montmorillonite were dispersed in 400g of water, stirred at 2000rpm for 2 hours at 30 ℃ and then dried to obtain 56g of hybrid montmorillonite.
The raw materials for preparing the emulsion comprise 56g of hybrid montmorillonite, 400g of 60# solid paraffin, 25g of propylene glycol monostearate and 17g of ethylene oxide monostearate.
The method for preparing the emulsion comprises the following steps:
1) the hybrid montmorillonite prepared as described above and 400g of 60# paraffin wax were mixed at 70 ℃ and 25g of propylene glycol monostearate, 17g of polyoxyethylene monostearate and 800g of water were added thereto and stirred at 5000rpm for 10min to prepare a complete primary emulsion.
2) Homogenizing the primary emulsion at 40MPa for 1 time by a high-pressure homogenizer to obtain the final product.
Example 2
This example relates to a paraffin-based Pickering emulsion containing hybrid montmorillonite.
The hybrid montmorillonite is prepared by the following method:
6g of gamma-aminopropyltriethoxysilane, 80g of ethyl orthosilicate, 80g of ethanol and 20g of sodium-based montmorillonite were dispersed in 300g of water, stirred at 3000rpm for 4 hours at 40 ℃ and then dried to obtain 32g of hybrid montmorillonite.
The raw materials for preparing the emulsion comprise 32g of the hybrid montmorillonite, 240g of 50# solid paraffin, 12g of sorbitan monooleate and 10g of polyoxyethylene monostearate.
The method for preparing the emulsion comprises the following steps:
1) the hybrid montmorillonite prepared as described above and 240g of 50# paraffin wax were mixed at 75 ℃, and 12g of sorbitan monooleate, 10g of polyoxyethylene monostearate and 600g of water were added thereto, and stirred at 7000rpm for 20min to prepare a complete primary emulsion.
2) Homogenizing the primary emulsion with a high-pressure homogenizer at 60MPa for 2 times to obtain the final product.
Example 3
This example relates to a paraffin-based Pickering emulsion containing hybrid montmorillonite.
The hybrid montmorillonite is prepared by the following method:
1g of gamma-glycidoxypropyltrimethoxysilane, 50g of propyl orthosilicate, 50g of n-propanol and 10g of calcium montmorillonite were dispersed in 100g of water, stirred at 4000rpm at 50 ℃ for 6 hours, and then dried to obtain 14g of hybrid montmorillonite.
The raw materials for preparing the emulsion comprise 14g of the hybrid montmorillonite, 100g of 15# liquid paraffin, 5g of polyoxyethylene dioleate and 3g of polyoxyethylene methyl glucoside hemioleate.
The method for preparing the emulsion comprises the following steps:
1) the hybrid montmorillonite prepared in the previous step and 100g of 15# liquid paraffin are mixed at 85 ℃, 5g of polyoxyethylene dioleate, 3g of polyoxyethylene methyl glucoside hemioleate and 200g of water are added into the mixture, and the mixture is stirred for 15min at the speed of 60000rpm to prepare a primary emulsion.
2) Homogenizing the primary emulsion at 80MPa for 1 time by a high-pressure homogenizer to obtain the final product.
Example 4
This example relates to a paraffin-based Pickering emulsion containing hybrid montmorillonite.
The hybrid montmorillonite is prepared by the following method:
10g of vinyltriethoxysilane, 200g of n-butyl orthosilicate, 200g of isopropanol and 50g of organic montmorillonite were dispersed in 500g of water, stirred at 6000rpm at 60 ℃ for 10 hours, and then dried to obtain 72g of hybrid montmorillonite.
The raw materials for preparing the emulsion comprise 72g of the hybrid montmorillonite, 500g of No. 5 liquid paraffin, 30g of sorbitan monooleate and 20g of polyoxyethylene sorbitan monooleate;
the method for preparing the emulsion comprises the following steps:
1) the hybrid montmorillonite prepared in the previous step and 500g of 5# liquid paraffin are mixed at 95 ℃, 30g of sorbitan monooleate, 20g of polyoxyethylene sorbitan monooleate and 1000g of water are added into the mixture, and the mixture is stirred at 10000rpm for 20min to prepare a primary emulsion.
2) Homogenizing the primary emulsion with a high-pressure homogenizer at 70MPa for 2 times to obtain the final product.
Comparative example 1
This comparative example relates to an emulsion which differs from example 1 in that no hybrid montmorillonite is added to it and in that it is prepared by a process comprising the following steps:
a preemulsion was prepared by mixing 240g of 50# paraffin wax, 12g of sorbitan monooleate, 10g of polyoxyethylene monostearate and 600g of water at 75 ℃ and stirring at 7000rpm for 20 min. And (3) homogenizing the primary emulsion for 2 times by a high-pressure homogenizer under the homogenizing pressure of 60MPa to obtain the paraffin-based Pickering emulsion wood emulsion.
Comparative example 2
This comparative example relates to an emulsion which differs from example 1 in that no hybrid montmorillonite is added to it and in that it is prepared by a process comprising the following steps:
a preemulsion was prepared by mixing 240g of 50# paraffin wax, 30g of sorbitan monooleate, 20g of polyoxyethylene monostearate and 600g of water at 75 ℃ and stirring at 7000rpm for 20 min. And (3) homogenizing the primary emulsion for 2 times by a high-pressure homogenizer under the homogenizing pressure of 60MPa to obtain the paraffin-based Pickering emulsion wood emulsion.
Experimental example 1
The emulsion wood emulsions in the examples were tested in 4 aspects of appearance, average particle size, centrifuge stability, and storage stability. The average particle size was measured using a Delsa Nano model C laser particle sizer. The method for measuring the centrifugal stability comprises the steps of respectively taking 10g of the emulsion wood emulsion used in the examples 1-4 and 10g of the paraffin-based Pickering emulsion wood emulsion used in the comparative examples 1-2, placing the emulsion wood emulsion in a centrifuge, centrifuging the mixture for 30min at the rotating speed of 3000r/min, and observing the stability of the emulsion. The results are shown in table 1:
TABLE 1
The results show that the particle size of all the examples is between 180nm and 250nm, and the centrifugal stability and the storage stability are kept good. The stability of comparative example 1 without the addition of the hybrid montmorillonite was significantly lower than that of the other examples, and better stability and lower particle size could be achieved only by increasing the surfactant content as shown in comparative example 2.
Experimental example 2
And (5) observing the adsorption condition of the hybrid montmorillonite on a paraffin/water interface by using TEM-EDX. Before observation, a proper amount of the emulsion wood waterproofing agent prepared in example 2 and the paraffin-based Pickering emulsion wood waterproofing agent prepared in comparative example 2 were dropped on a copper mesh containing a carbon film. After the water is evaporated, the adsorption condition of the hybrid montmorillonite around the liquid drops is observed. The results are shown in FIG. 1.
The emulsion droplets are distributed in a spherical shape, and in the traditional paraffin-based Pickering emulsion (comparative example 2, FIG. 1a) without the addition of the hybrid montmorillonite, the hybrid montmorillonite is not adsorbed on the surfaces of the droplets. However, the surface of the emulsion wood waterproofing agent (example 2, FIG. 1b and FIG. 1c) drop has obvious black solid substance, and the energy spectrum scan of FIG. 1c shows that the black substance is the hybrid montmorillonite particle containing Si element. The hybrid montmorillonite particles can be adsorbed on the surface of the liquid drops, the mechanical barrier and electrostatic repulsion between the liquid drops are improved by utilizing the solid particle film layer, and the stability of the emulsion is improved.
Experimental example 3
The emulsion wood water repellent used in examples 1 to 4 and the paraffin-based Pickering emulsion wood water repellent of comparative example 2 were each diluted to a solid content of 2%, followed by impregnation of aspen having a size of 20 mm. times.20 mm. The processing method comprises the following steps: putting the wood into an impregnation tank, firstly carrying out vacuum treatment under the vacuum degree of-0.9 MPa for 30min, then stopping vacuum, adding the diluted emulsion into the impregnation tank, and pressurizing for 60min under the condition of 2 MPa. After the vacuum pressure impregnation is completed, the wood is taken out from the impregnation tank and air-dried. In addition, untreated poplars were taken as a blank group.
Subsequently, with reference to GB/T1934.1-2009 "method for determining Water absorption of Wood", the water absorption of wood was measured for 24 h; measuring the volume expansion rate of the wood for 24 hours by referring to GB/T1934.2-2009 Wood swelling capacity determination method; the bending elastic modulus and the bending strength of the wood are measured by referring to GB1936.1-1991 method for measuring the bending elastic modulus of the wood and GB 1936.2 method for testing the bending strength of the wood; reference is made to GB/T2406.2-2009 section 2 for determination of the burning behaviour of plastics by oxygen index method: room temperature test "measures the oxygen index of wood. The results are shown in Table 2.
TABLE 2 physical and mechanical Properties of the treated Density fiberboard
The result shows that the water absorption and volume expansion rate of the wood can be obviously reduced by adopting the emulsion wood waterproofing agent prepared by the invention to treat the wood, the good hydrophobicity and size stability are shown, and the effect is better than that of the traditional paraffin-based Pickering emulsion without adding hybrid montmorillonite (comparative example 2). The traditional paraffin-based Pickering emulsion (comparative example 2) without adding hybrid montmorillonite can not improve the mechanical properties of wood such as bending strength, elastic modulus and the like, and even can reduce the oxygen index of wood, so that the wood is more flammable. The emulsion wood waterproofing agent can obviously improve the mechanical property and the flame retardant property of the wood.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The paraffin-based Pickering emulsion containing hybrid montmorillonite is characterized in that the raw materials for preparing the emulsion contain the hybrid montmorillonite, and the hybrid montmorillonite is prepared by modifying montmorillonite with silane, micromolecular alcohol and silicate ester;
the mass ratio of the silane to the silicate to the micromolecular alcohol to the montmorillonite is 1-2: 12-50: 12-50: 3-10;
the silicate is one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate;
the hybrid montmorillonite is prepared by the following method:
montmorillonite, silane, micromolecular alcohol and silicate ester are mixed and stirred for 2 to 10 hours at the temperature of between 30 and 60 ℃ and at the speed of 2000-6000 rpm;
the raw materials for preparing the paraffin emulsion also comprise paraffin, a low HLB value nonionic surfactant and a high HLB value nonionic surfactant;
the low HLB value nonionic surfactant is one or more of propylene glycol monostearate, glyceryl monostearate, polyoxypropylene stearate, tetraethylene glycol monostearate, polyoxyethylene dioleate, sorbitan monooleate or sorbitan monooleate;
the high HLB value nonionic surfactant is one or more of polyoxyethylene monostearate, polyoxyethylene cetyl alcohol, polyoxyethylene sorbitan monooleate, polyoxyethylene monolaurate or polyoxyethylene methyl glucoside hemioleate;
the paraffin-based Pickering emulsion is prepared by the following method:
1) mixing the hybrid montmorillonite and paraffin at 70-95 ℃, adding a low HLB value nonionic surfactant and a high HLB value nonionic surfactant, and stirring at 5000-10000 rpm for 10-20min to prepare a primary emulsion;
2) and (3) homogenizing the primary emulsion for 1-2 times by a high-pressure homogenizer under the homogenizing pressure of 40-80 MPa to obtain the paraffin-based Pickering emulsion.
2. The paraffin-based Pickering emulsion according to claim 1, wherein the silane is one or more of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltriethoxysilane, or vinyltris (beta-methoxyethoxy) silane.
3. The paraffin-based Pickering emulsion according to claim 2, wherein the silane is gamma-aminopropyltrimethoxysilane or gamma-aminopropyltriethoxysilane.
4. The paraffin-based Pickering emulsion according to claim 1, wherein the montmorillonite is one or more of sodium montmorillonite, calcium montmorillonite or organic montmorillonite;
and/or the small molecular alcohol is one or more of methanol, ethanol, n-propanol or isopropanol.
5. The paraffin-based Pickering emulsion according to claim 4, wherein the small molecule alcohol is ethanol.
6. The paraffin-based Pickering emulsion according to claim 1, wherein the paraffin is liquid paraffin or solid paraffin;
and/or the low HLB nonionic surfactant is sorbitan monooleate and sorbitan monooleate;
and/or the high HLB nonionic surfactant is polyoxyethylene monostearate or polyoxyethylene monolaurate.
7. The paraffin-based Pickering emulsion according to claim 6, wherein the paraffin is No. 5 liquid paraffin or No. 50 solid paraffin.
8. The paraffin-based Pickering emulsion according to any one of claims 1 to 7, wherein when the amount of water is 1L, the raw materials for preparing the paraffin-based Pickering emulsion comprise 10 to 80g of hybrid montmorillonite, 200 to 700g of paraffin, 10 to 50g of low HLB value nonionic surfactant and 10 to 40g of high HLB value nonionic surfactant.
9. The paraffin-based Pickering emulsion according to any one of claims 1 to 7, wherein when the amount of water is 1L, the raw materials for preparing the paraffin-based Pickering emulsion comprise 50 to 70g of hybrid montmorillonite, 400 to 500g of paraffin, 20 to 32g of low HLB value nonionic surfactant and 15 to 25g of high HLB value nonionic surfactant.
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| CN111087538B (en) * | 2020-01-02 | 2021-02-05 | 中国科学院长春应用化学研究所 | W/O emulsion and preparation method thereof, polymer particles and preparation method thereof |
| CN112157770B (en) * | 2020-10-15 | 2022-02-01 | 南京林业大学 | Environment-friendly type bamboo wood mildew-proof treatment method |
| CN114395387B (en) * | 2022-03-15 | 2022-12-20 | 西南石油大学 | Water-in-oil in-situ emulsified nano oil displacement agent with high phase transition point and application thereof |
| CN115414262B (en) * | 2022-07-19 | 2023-09-22 | 江苏诺兴生物科技有限公司 | Epsilon-polylysine Pickering emulsion and preparation method and application thereof |
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