CN103320003A - Preparation method for nanometer cellulose composite waterborne polyurethane paint film on wood surface - Google Patents
Preparation method for nanometer cellulose composite waterborne polyurethane paint film on wood surface Download PDFInfo
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- CN103320003A CN103320003A CN2013102942328A CN201310294232A CN103320003A CN 103320003 A CN103320003 A CN 103320003A CN 2013102942328 A CN2013102942328 A CN 2013102942328A CN 201310294232 A CN201310294232 A CN 201310294232A CN 103320003 A CN103320003 A CN 103320003A
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Abstract
The invention provides a preparation method for a nanometer cellulose composite waterborne polyurethane paint film on a wood surface, which relates to a preparation method for a wood surface paint film. The invention aims to overcome the problems of severe pollution to the environment, high toxicity and low strength of a conventional wood surface paint film. The method comprises the following steps: 1, preparation of nanometer cellulose; 2, synthesis of a waterborne polyurethane emulsion; and 3, preparation of the nanometer cellulose composite waterborne polyurethane paint film on the wood surface. The preparation method is simple, easy to operate, environment-friendly, safe and nontoxic; Young modulus is increased by 32%, which proves strength of the waterborne polyurethane paint film is enhanced indeed; temperature corresponding to a maximum weight loss rate is 420 DEG C, which shows that heat stability of a Korean pine chip is obviously improved after the polyurethane paint film is coated on the surface of the chip.
Description
Technical field
The present invention relates to a kind of preparation method of wood surface paint film.
Background technology
Coat the effect that one deck paint film can play to timber protection and prolonging wood using life at wood surface.Contain a large amount of organic solvents in the solvent borne polyurethane, organic solvent is poisonous, and serious environment pollution, and especially solvent residual amount is very high in two component polyurethane, and has high toxicity.
Aqueous polyurethane refers to mainly replace organic solvent with water as reaction solvent in preparation urethane process.Distinguish by exterior appearance, aqueous polyurethane is broadly divided into 3 classes: polyurethane dispersing liquid, aqueous polyurethane, polyaminoester emulsion.Differentiation is the form of water-dispersion in the polyurethane macromolecular particle, does not have definite restriction, and said aqurous ployurethane refers to polyurethane dispersions or aqueous polyurethane emulsion in the real life production.Adopt at present aqueous polyurethane as the wood surface paint film, exist paint film intensity to hang down problem.
Summary of the invention
The present invention seeks to solve and adopt solvent borne polyurethane to have serious environment pollution, problem that toxicity is high as the wood surface paint film, adopt aqueous polyurethane to have the low problem of paint film intensity as the wood surface paint film, and a kind of preparation method of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film is provided.
The preparation method of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film, realize according to the following steps:
One, the preparation of nano-cellulose: be pre-treatment 2～4h in 30%～60% the sulphuric acid soln at massfraction with 1.00～3.00g bamboo pulp, filtering and washing is to neutral, then product is distributed in 400～500mL deionized water, join behind ultra-sonic dispersion 5～10min and grind 0.5～1h in the colloidal mill, join again in the high pressure homogenizer, homogeneous is 10～20 times under the pressure of 1000～1500Bar, then product is carried out cytoclasis 5～15min, obtains nano-cellulose colloidal solution;
Two, synthesizing of aqueous polyurethane emulsion: 50～150mL acetone is joined in the beaker that fills 10～30g polyoxyethylene glycol, add until completely dissolved the 3.5g tolylene diisocyanate, splash into 3～5 dibutyl tin laurates, then solution is transferred to reflux condensing tube, in the there-necked flask of mechanical stirrer, at 70～90 ℃ of lower reaction 1～1.5h, obtain Waterborne Polyurethane Prepolymer, cool the temperature to 60 ℃, to wherein adding 0.62g diethylenetriamine and 0.22g glycol ether, reaction 2～4h cools the temperature to 45 ℃, add Glacial acetic acid 0.3g, reaction 0.5h cools the temperature to 20 ℃ again, adds 50～150mL distilled water, be stirred to emulsification, then transfer in the Rotary Evaporators, steam acetone, obtain aqueous polyurethane emulsion;
Three, the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film: be to mix at 4: 1 by volume with aqueous polyurethane emulsion and nano-cellulose colloidal solution, magnetic agitation obtains mixture system, then pending wood chip is put into mixture system and soak 20～26h, dry under the room temperature after taking out, namely finish the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film.
The invention has the advantages that:
1, by pre-polymerization, chain extension, neutralization, emulsification and rotary evaporation, make stable aqueous polyurethane emulsion, then via the physical blending method the high-pressure homogeneous nano-cellulose that makes is incorporated in this emulsion system.At wood surface coated with nano Mierocrystalline cellulose composite aqueous polyurethane paint film.Method is simple, and is easy to operate, environmental friendliness, safety non-toxic.
2, red pine wood chips, the red pine wood chips that scribbles aqueous polyurethane and gained surface-coated of the present invention have the red pine wood chips of nano-cellulose composite aqueous polyurethane paint film, Young's modulus is followed successively by 71569MPa, 45448MPa, 60175MPa, can draw thus after applying the aqueous polyurethane paint film, the Young's modulus of wood chip descends to some extent, and the red pine wood chips of nano-cellulose composite aqueous polyurethane paint film is arranged in surface-coated, Young's modulus has increased 32%, illustrates that the introducing of nano-cellulose has strengthened the intensity of aqueous polyurethane paint film really.
3, can find out by DTG figure, the temperature that the maximum weight loss rate of red pine wood chips is corresponding is 382 ℃, and scribble the red pine wood chips of aqueous polyurethane and the red pine wood chips that gained surface-coated of the present invention has nano-cellulose composite aqueous polyurethane paint film, temperature corresponding to maximum weight loss rate is 420 ℃, illustrated that after Polyurethane lacquer was coated on the red pine wood chips surface, its thermostability had obviously improved.
Description of drawings
Fig. 1 is the Fourier transform infrared spectrogram that the gained surface-coated has the red pine wood chips of nano-cellulose composite aqueous polyurethane paint film among the embodiment;
Fig. 2 is the scanning electron microscope diagram of sample a among the embodiment;
Fig. 3 is the scanning electron microscope diagram of sample b among the embodiment;
Fig. 4 is the scanning electron microscope diagram of sample c among the embodiment;
Fig. 5 is the fracture figure of sample a, b and c among the embodiment;
Fig. 6 is the stress-strain curve diagram of sample a, b and c among the embodiment;
Fig. 7 is the TG graphic representation of sample a, b and c among the embodiment;
Fig. 8 is the DTG graphic representation of sample a, b and c among the embodiment.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film, realize according to the following steps:
One, the preparation of nano-cellulose: be pre-treatment 2～4h in 30%～60% the sulphuric acid soln at massfraction with 1.00～3.00g bamboo pulp, filtering and washing is to neutral, then product is distributed in 400～500mL deionized water, join behind ultra-sonic dispersion 5～10min and grind 0.5～1h in the colloidal mill, join again in the high pressure homogenizer, homogeneous is 10～20 times under the pressure of 1000～1500Bar, then product is carried out cytoclasis 5～15min, obtains nano-cellulose colloidal solution;
Two, synthesizing of aqueous polyurethane emulsion: 50～150mL acetone is joined in the beaker that fills 10～30g polyoxyethylene glycol, add until completely dissolved the 3.5g tolylene diisocyanate, splash into 3～5 dibutyl tin laurates, then solution is transferred to reflux condensing tube, in the there-necked flask of mechanical stirrer, at 70～90 ℃ of lower reaction 1～1.5h, obtain Waterborne Polyurethane Prepolymer, cool the temperature to 60 ℃, to wherein adding 0.62g diethylenetriamine and 0.22g glycol ether, reaction 2～4h cools the temperature to 45 ℃, add Glacial acetic acid 0.3g, reaction 0.5h cools the temperature to 20 ℃ again, adds 50～150mL distilled water, be stirred to emulsification, then transfer in the Rotary Evaporators, steam acetone, obtain aqueous polyurethane emulsion;
Three, the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film: be to mix at 4: 1 by volume with aqueous polyurethane emulsion and nano-cellulose colloidal solution, magnetic agitation obtains mixture system, then pending wood chip is put into mixture system and soak 20～26h, dry under the room temperature after taking out, namely finish the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film.
Bamboo pulp is the paper pulp for preparing take bamboo as raw material in the paper mill in the present embodiment step 1.
Nano-cellulose colloidal solution in the present embodiment step 1 obtains the solid nano Mierocrystalline cellulose after lyophilize, for subsequent use.
Remaining mixture system in the present embodiment step 3 behind the pending wood chip of immersion, by lyophilize, the solid that obtains, for subsequent use.
Pending wood chip is the timber that cuts into desired size and will prepare on the surface nano-cellulose composite aqueous polyurethane paint film in the present embodiment step 3.
Embodiment two: present embodiment and embodiment one are different is to be pre-treatment 3h in 45% the sulphuric acid soln with 2.00g bamboo pulp at massfraction in the step 1.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment one or two is that product is distributed in the 450mL deionized water in the step 1, join behind the ultra-sonic dispersion 8min and grind 0.7h in the colloidal mill, join again in the high pressure homogenizer, homogeneous is 15 times under the pressure of 1200Bar, then product is carried out cytoclasis 10min.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three is that tolylene diisocyanate and polyoxyethylene glycol need before use respectively at 40～50 ℃ of lower processed 10～16h in the step 2.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is in the step 2 100mL acetone to be joined in the beaker that fills the 20g polyoxyethylene glycol.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: what present embodiment was different from one of embodiment one to five is to splash into 4 dibutyl tin laurates in the step 2.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is at 80 ℃ of lower reaction 1.2h in the step 2.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is in the step 2 pending wood chip to be put into mixture system to soak 24h.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight is that the rotating speed of magnetic agitation in the step 3 is 600r/min, and churning time is 1.5h.Other step and parameter are identical with one of embodiment one to eight.
Embodiment:
The preparation method of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film, realize according to the following steps:
One, the preparation of nano-cellulose: be pre-treatment 2h in 30% the sulphuric acid soln at massfraction with 2.00g bamboo pulp, filtering and washing is to neutral, then product is distributed in the 450mL deionized water, join behind the ultra-sonic dispersion 5min and grind 0.5h in the colloidal mill, join again in the high pressure homogenizer, homogeneous is 15 times under the pressure of 1500Bar, then product is carried out cytoclasis 10min, obtains nano-cellulose colloidal solution;
Two, synthesizing of aqueous polyurethane emulsion: 100mL acetone is joined in the beaker that fills the 20g polyoxyethylene glycol, add until completely dissolved the 3.5g tolylene diisocyanate, splash into 4 dibutyl tin laurates, then solution is transferred to reflux condensing tube, in the there-necked flask of mechanical stirrer, at 80 ℃ of lower reaction 1.5h, obtain Waterborne Polyurethane Prepolymer, cool the temperature to 60 ℃, to wherein adding 0.62g diethylenetriamine and 0.22g glycol ether, reaction 2～4h cools the temperature to 45 ℃, add Glacial acetic acid 0.3g, reaction 0.5h cools the temperature to 20 ℃ again, adds 100mL distilled water, be stirred to emulsification, then transfer in the Rotary Evaporators, steam acetone, obtain aqueous polyurethane emulsion;
Three, the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film: be to mix at 4: 1 by volume with aqueous polyurethane emulsion and nano-cellulose colloidal solution, magnetic agitation obtains mixture system, then pending wood chip is put into mixture system and soak 24h, dry under the room temperature after taking out, namely finish the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film.
Tolylene diisocyanate and polyoxyethylene glycol need before use respectively at 45 ℃ of lower processed 12h in the present embodiment step 2.
Pending wood chip is long 120mm in the present embodiment step 3, wide 15mm, the red pine wood chips of thick 0.341mm.
The present embodiment gained surface-coated has the red pine wood chips of nano-cellulose composite aqueous polyurethane paint film, its Fourier transform infrared spectrogram, as shown in Figure 1, NCC is nano-cellulose, WPU is the aqueous polyurethane solid, and WPU/NCC is nano-cellulose composite aqueous polyurethane solid.On the NCC spectrogram, can see 3300cm
-1Near absorption peak is-the OH stretching vibration peak 1050cm
-1Near absorption peak is the C-O-C stretching vibration peak.Contrast WPU and WPU/NCC spectrogram can find out that both almost do not have difference, illustrate that nano-cellulose has well been wrapped up by aqueous polyurethane, and its collection of illustrative plates does not embody in compound system, and 2300cm
-1About do not have the absorption peak of appearance-NCO, illustrate in the raw material-NCO participated in reaction fully; Simultaneously, 1735cm
-1The C=O absorption peak of obvious carbamate has appearred in the place, illustrates really to have generated carbamate, in addition 2900cm
-1About the methylene radical absorption peak, 1450～1600cm
-1The stretching vibration peak of phenyl ring basic framework also all in spectrogram, significantly embodied out.
Blank reference: red pine wood chips, i.e. sample a; Its scanning electron microscope diagram, as shown in Figure 2.
Contrast experiment: replace nano-cellulose colloidal solution with deionized water, scribble the red pine wood chips of aqueous polyurethane, i.e. sample b; Its scanning electron microscope diagram, as shown in Figure 3.
The present embodiment gained surface-coated has the red pine wood chips of nano-cellulose composite aqueous polyurethane paint film, i.e. sample c; Its scanning electron microscope diagram, as shown in Figure 4.
On Fig. 2, can see very clearly the lines pit of red pine wood chips, comparison diagram 3 and Fig. 4 are as can be known, on red pine wood chips, really scribble one deck paint film, coating surface has jog on Fig. 3, than unfairness, paint film is then more smooth on Fig. 4, and viscosity is also obviously greater than Fig. 3, the interpolation that nano-cellulose is described can be played certain thickening power to aqueous polyurethane really, and can make sample surfaces more smooth.
The fracture figure of sample a, b and c, as shown in Figure 5, in drawing process, obvious moulding distortion does not appear in sample before fracture, so all belong to brittle rupture; The appearance of fracture that sample a occurs is because in drawing process, sample may be because thinner cause, directly occured to tear along the pit lines, sample b and sample c then be since the aqueous polyurethane paint film to be coated in the wood chip surface be the pit lines that has directly stopped up wood chip itself, brittle failure has occured in loading process.
The stress-strain(ed) curve of sample a, b and c, as shown in Figure 6, stress-strain(ed) curve can be obtained, and the Young's modulus of sample a, b and c is followed successively by 71569MPa, 45448MPa, 60175MPa, can draw thus after applying the aqueous polyurethane paint film, the Young's modulus of wood chip descends to some extent, and the red pine wood chips of nano-cellulose composite aqueous polyurethane paint film is arranged in surface-coated, Young's modulus has increased 32%, illustrates that the introducing of nano-cellulose has strengthened the intensity of aqueous polyurethane paint film really.
The TG curve of sample a, b and c as shown in Figure 7, can be found out from TG figure, and the thermogravimetric curve of sample all is three phases, and the fs is 50～150 ℃; Concerning a, this stage belongs to the dehydration stage, and for b, c, may also comprise the volatilization of the organic molecule that adsorbs in the aqueous polyurethane in the time of dehydration.Subordinate phase is 150～290 ℃, and this stage is platform, and weightlessness does not occur sample, and quality is kept constant substantially.Phase III is 290～470 ℃, and this stage mainly is the decomposition of sample, during be accompanied by losing of hydrogen-oxygen atom and part carbon atom, sample is weightless very fast.After 470 ℃, reaction finishes, and residual volume remains unchanged substantially.
The DTG curve of sample a, b and c, as shown in Figure 8, can find out by DTG figure, temperature corresponding to the maximum weight loss rate of a sample is 382 ℃, and temperature corresponding to the maximum weight loss rate of b, c sample is 420 ℃, illustrated that after Polyurethane lacquer was coated on the red pine wood chips surface, its thermostability had obviously improved, and whether little on its thermostability impact the interpolation of nano-cellulose is.
Claims (9)
1. the preparation method of a wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film is characterized in that it realizes according to the following steps:
One, the preparation of nano-cellulose: be pre-treatment 2～4h in 30%～60% the sulphuric acid soln at massfraction with 1.00～3.00g bamboo pulp, filtering and washing is to neutral, then product is distributed in 400～500mL deionized water, join behind ultra-sonic dispersion 5～10min and grind 0.5～1h in the colloidal mill, join again in the high pressure homogenizer, homogeneous is 10～20 times under the pressure of 1000～1500Bar, then product is carried out cytoclasis 5～15min, obtains nano-cellulose colloidal solution;
Two, synthesizing of aqueous polyurethane emulsion: 50～150mL acetone is joined in the beaker that fills 10～30g polyoxyethylene glycol, add until completely dissolved the 3.5g tolylene diisocyanate, splash into 3～5 dibutyl tin laurates, then solution is transferred to reflux condensing tube, in the there-necked flask of mechanical stirrer, at 70～90 ℃ of lower reaction 1～1.5h, obtain Waterborne Polyurethane Prepolymer, cool the temperature to 60 ℃, to wherein adding 0.62g diethylenetriamine and 0.22g glycol ether, reaction 2～4h cools the temperature to 45 ℃, add Glacial acetic acid 0.3g, reaction 0.5h cools the temperature to 20 ℃ again, adds 50～150mL distilled water, be stirred to emulsification, then transfer in the Rotary Evaporators, steam acetone, obtain aqueous polyurethane emulsion;
Three, the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film: be to mix at 4: 1 by volume with aqueous polyurethane emulsion and nano-cellulose colloidal solution, magnetic agitation obtains mixture system, then pending wood chip is put into mixture system and soak 20～26h, dry under the room temperature after taking out, namely finish the preparation of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film.
2. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 1 is characterized in that in the step 1 that be pre-treatment 3h in 45% the sulphuric acid soln with 2.00g bamboo pulp at massfraction.
3. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 1 and 2, it is characterized in that product is distributed in the 450mL deionized water in the step 1, join behind the ultra-sonic dispersion 8min and grind 0.7h in the colloidal mill, join again in the high pressure homogenizer, homogeneous is 15 times under the pressure of 1200Bar, then product is carried out cytoclasis 10min.
4. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 3, it is characterized in that tolylene diisocyanate and polyoxyethylene glycol need before use respectively at 40～50 ℃ of lower processed 10～16h in the step 2.
5. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 4 is characterized in that in the step 2 100mL acetone being joined in the beaker that fills the 20g polyoxyethylene glycol.
6. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 5 is characterized in that splashing in the step 24 dibutyl tin laurates.
7. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 6 is characterized in that in the step 2 at 80 ℃ of lower reaction 1.2h.
8. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 7 is characterized in that in the step 2 pending wood chip being put into mixture system soaks 24h.
9. the preparation method of a kind of wood surface nano Mierocrystalline cellulose composite aqueous polyurethane paint film according to claim 8, the rotating speed that it is characterized in that magnetic agitation in the step 3 is 600r/min, churning time is 1.5h.
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