CN105256549A - Preparation method of bamboo fibers with low releasing of organic volatile matters - Google Patents
Preparation method of bamboo fibers with low releasing of organic volatile matters Download PDFInfo
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- CN105256549A CN105256549A CN201510751572.8A CN201510751572A CN105256549A CN 105256549 A CN105256549 A CN 105256549A CN 201510751572 A CN201510751572 A CN 201510751572A CN 105256549 A CN105256549 A CN 105256549A
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- 239000000835 fiber Substances 0.000 title claims abstract description 97
- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 92
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 92
- 241001330002 Bambuseae Species 0.000 title claims abstract description 92
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 92
- 239000011425 bamboo Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000012948 isocyanate Substances 0.000 claims abstract description 37
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000003607 modifier Substances 0.000 claims description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- WHIVNJATOVLWBW-UHFFFAOYSA-N n-butan-2-ylidenehydroxylamine Chemical compound CCC(C)=NO WHIVNJATOVLWBW-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000839 emulsion Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 8
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 8
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- IVKNZCBNXPYYKL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO)C=C1 IVKNZCBNXPYYKL-UHFFFAOYSA-N 0.000 claims description 4
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical compound N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 claims 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
- 238000004132 cross linking Methods 0.000 abstract description 6
- 239000012802 nanoclay Substances 0.000 abstract description 6
- 229920002488 Hemicellulose Polymers 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 229920005610 lignin Polymers 0.000 abstract description 3
- 239000012855 volatile organic compound Substances 0.000 abstract 2
- 238000003672 processing method Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 24
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 15
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000001514 detection method Methods 0.000 description 8
- 150000001299 aldehydes Chemical class 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- CKXFVRQVHVLLGH-UHFFFAOYSA-N CC(CC)=NO.C(CCCCCN=C=O)N=C=O Chemical compound CC(CC)=NO.C(CCCCCN=C=O)N=C=O CKXFVRQVHVLLGH-UHFFFAOYSA-N 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 5
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000004744 fabric Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- -1 aliphatic isocyanates Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention discloses a preparation method of bamboo fibers with low releasing of organic volatile matters, aiming at improving the cross-linking degree of all components of the bamboo fibers so as to reduce the releasing of the organic volatile matters, caused by high-temperature decomposition, of the bamboo fibers with low releasing of organic volatile matters. With the adoption of the method for improving the cross-linking degree of all the components of the bamboo fibers through enclosed type isocyanate to increase the decomposition temperature of all the components of the bamboo fibers, the decomposition temperature is higher than that of a processing method, so that the aim of reducing the releasing of the organic volatile matters is realized; lignin and hemicellulose components capable of improving the mechanical properties of the bamboo fibers are kept in the bamboo fibers; and meanwhile, nano clay which possibly causes a dispersion problem is not used so that the releasing of VOC (Volatile Organic Compounds) of the bamboo fibers is improved basically.
Description
Technical field
The present invention relates to bamboo fibre field, specifically, be a kind of low VOC release bamboo fibre preparation method, improve each component cross-link degree of bamboo fibre thus reduce its pyrolytic volatile organic matter release low VOC release bamboo fibre.
Background technology
The plant material of occurring in nature is the renewable resource that resource is the abundantest.Natural plant fibre extracts by plant material the fiber obtained.Natural plant fibre reaches 26.5 × 10^10t in the total amount of occurring in nature, existing petroleum total reserve on the earth.Therefore, one of the green material of natural plant fibre alternatively fossil energy derivative products, obtains society and researcher more and more payes attention to.And bamboo has as a kind of the natural fiber source distributed widely in China, enter rapidly the visual field of people, bamboo fibre is also subject to people and more and more pays close attention to.
But in the application of reality, the organic volatile of bamboo fiber products, especially acetaldehyde exceeds standard and seriously constrains its application in the field such as fitment material for family, automotive interior material.In bamboo fibre composition, except the cellulose components having heat resistance stable, also comprise the hemicellulose and the composition such as pectin that start at a lower temperature to decompose, and these compositions also just bamboo fibre by the main cause volatilizing aldehyde material in hot procedure.
The method that CN103774243 is rubbed by cal rolling removes pectin in natural fabric and hemicellulose components to reduce its aldehydes volatilization in thermoforming process, but in the process that cal rolling is rubbed, often cause the major injury of natural fabric, its mechanical property is reduced greatly.CN104690979 and CN103774344A is then subject to thermogenetic aldehydes and benzene class material by nano-clays adsorb natural fabric, to prepare the natural-fiber composite material of low VOC release; But the absorption of nanoclay belongs to physical absorption, therefore there is the absorption limit, in the field that natural fabric use amount is higher, often need to add a large amount of nanoclay to reach the requirement of low VOC release, add the problem that nanoclay then can bring such as nanoparticle dispersion difficulty etc. new in a large number.
Summary of the invention
The present invention is just for the improvement done by prior art, there is provided a kind of improve each component cross-link degree in bamboo fibre by blocked isocyanate thus improve the method for each decomposition of components temperature of bamboo fibre, make its decomposition temperature higher than processing temperature, thus reach the object reducing organic volatile release, both in bamboo fibre, lignin, the hemi-cellulose components that can improve bamboo fibre mechanical property had been remained, also avoid using the nanoclay that may bring scattering problem, be the VOC release fundamentally improving bamboo fibre simultaneously.
The present invention is achieved through the following technical solutions:
A preparation method for low VOC release bamboo fibre, preparation method comprises the following steps successively:
1), by bamboo fibre rinsing in water, and be dried to constant weight, baking temperature is 60 DEG C-110 DEG C, because drying is a longer process, therefore temperature is unsuitable too high, and limiting temperature can energy efficient, as long as carry out efficient drying to bamboo fibre;
2), surfactant is added to the water, be configured to the aqueous solution that concentration is 5g/L-50g/L, continue stirring until surfactant to dissolve completely, surfactant is mainly used in blocked isocyanate to be scattered in water, forms stable emulsion, but addition is unsuitable too low too high, addition is too low then cannot limited dispersion blocked isocyanate, the too high one side of addition causes waste, exhibiting high surface activating agent then can be caused on bamboo fibre surface on the one hand to remain, affect its heat endurance;
3), under Keep agitation, to step 2) add blocked isocyanate in gained solution, blocked isocyanate addition is step 2) 2%-8% of described aqueous solution quality, stir 10 minutes-30 minutes under 800-1200 rev/min of mixing speed, obtain emulsion, be designated as modifier, limit herein blocked isocyanate consumption be because, if consumption is too low, then cannot at the enough blocked isocyanate of bamboo fibre adsorption, if too high levels, then, after immersion, drying and heat treatment, the adhesion between fiber can be caused; Limit mixing time be because, if mixing time is too short, stable emulsion cannot be formed, the long necessity also do not had very of mixing time, therefore the blocked isocyanate of 2%-8% mass fraction and the mixing time of 10 minutes-30 minutes are the data areas of optimum technical solution of the present invention;
4), by bamboo fibre step 3 is immersed) gained modifier, and continue immersion 5 ~ 30 minutes, then sieving leaches bamboo fibre, and is dried to constant weight at 60 DEG C-80 DEG C by the bamboo fibre leached; Limiting time is because if the time is too short, the amount of bamboo fibre adsorption isocyanates is inadequate, if overlong time, resource of losing time, does not have necessity very;
5), by step 4) gained bamboo fibre carries out the heat treatment of 30 minutes-2 hours at 120 DEG C of-180 DEG C of temperature, can obtain low VOC release bamboo fibre.Defined reaction temperature is that too low, cannot dissociate generation isocyanate groups, too high, can impact properties of bamboo because dissociating of blocked isocyanate sealer needs certain temperature.
As improving further, step 2 of the present invention) in, surfactant is the mixture of any one or any two kinds in dodecyl phenenyl sulfate, lauryl sodium sulfate, OP-10, polysorbas20.
As improving further, step 3 of the present invention) in, blocked isocyanate is for adopting sodium hydrogensulfite, methyl ethyl ketoxime, acetylacetone,2,4-pentanedione, any one enclosed type hexamethylene diisocyanate (HDI) as sealer gained in epsilon-caprolactams or toluene di-isocyanate(TDI) (TDI) or methyl diphenylene diisocyanate (MDI), in the early stage in the dry run of 60 DEG C, isocyanates does not react with hydrone, because a large amount of isocyanates can be consumed with water molecule reaction affect and improve effect, and after dry run completes, heat up further again, the hydroxy-containing component that isocyanates is able to smoothly and in bamboo fibre reacts, form a large amount of cross-linked structures, improve component heat endurance, reduce the release of VOC in bamboo fibre heat treatment process, so the sequence arrangement between the selection of technological means and each technological means is also vital.
As improving further, blocked isocyanate of the present invention is the hexamethylene diisocyanate that methyl ethyl ketoxime closes end group.
As improving further, step 3 of the present invention) in, preferred blocked isocyanate addition is step 2) 4%-6% of described aqueous solution quality.
The invention has the beneficial effects as follows:
Improve each component cross-link degree in bamboo fibre with crosslinking agent thus improve the method for each decomposition of components temperature of bamboo fibre, make its decomposition temperature higher than processing temperature, thus reach the object reducing organic volatile release, both in bamboo fibre, remain the lignin component that can improve bamboo fibre mechanical property, also avoid using the nanoclay that may bring scattering problem, be the VOC release fundamentally improving bamboo fibre simultaneously.Meanwhile, the water-based system that the present invention adopts it also avoid the secondary pollution problem with an organic solvent brought.
Detailed description of the invention
The invention discloses the preparation method of a kind of low VOC release bamboo fibre, bamboo fibre is in immersion blocked isocyanate emulsion and after sieving and leaching surplus liquid, the blocked isocyanate disperseed in emulsion can be adsorbed in bamboo fibre surface, simultaneously, because baking temperature is after this lower namely 60 DEG C, therefore, in this dry run, blocked isocyanate can't react with the component of hydroxyl in bamboo fibre.And in the heat treatment process of follow-up higher temperature (120 DEG C-180 DEG C), sealer can dissociate from terminal isocyanate groups by Yin Gaowen, thus release isocyanate groups, and isocyanate groups just can react with the hydroxy-containing component in bamboo fibre.Owing to have employed blocked isocyanate, can ensure in the dry run of 60 DEG C in the early stage, isocyanates does not react with hydrone, because a large amount of isocyanates can be consumed with water molecule reaction affect and improve effect, and after dry run completes, heat up further again, NCO group in isocyanates can be reacted with the hydroxy-containing component in bamboo fibre, so can cross-linked structure be formed or form the higher component of molecular weight after react with hydroxy-containing component, thus improve its heat endurance, reduce the release of bamboo fibre VOC in heat treatment process.
Below in conjunction with specific embodiment, technical scheme of the present invention is described further:
Embodiment 1
A preparation method for low VOC release bamboo fibre, comprises the following steps successively:
1), by bamboo fibre rinsing in water, be then dried to constant weight, baking temperature is 60 DEG C;
2), by lauryl sodium sulfate be added to the water, be configured to the aqueous solution that concentration is 15g/L, continue stirring until lauryl sodium sulfate and dissolve completely;
3), under Keep agitation, to step 2) add the hexamethylene diisocyanate that methyl ethyl ketoxime closes end group in gained solution, the hexamethylene diisocyanate addition that methyl ethyl ketoxime closes end group is 5% of aqueous solution quality, stir 30 minutes under 1000 revs/min of mixing speeds, obtain emulsion, be designated as modifier;
4), by bamboo fibre step 3 is immersed) gained modifier, and continue immersion 30 minutes, then sieving leaches bamboo fibre, and is dried to constant weight at 60 DEG C by the bamboo fibre leached;
5), by step 4) gained bamboo fibre carries out the heat treatment of 30 minutes at 160 DEG C of temperature, can obtain low VOC release bamboo fibre.
Get the low VOC release bamboo fibre obtained in 100g embodiment 1 and process 15 minutes in 210 DEG C of baking ovens, be then placed on 23 ± 2 DEG C, 24h in 50 ± 5%RH environment.Sample is put into 10L sampler bag, be filled with 5L high pure nitrogen, 60 DEG C are heated 2h ± 2min in VOC samples storehouse.After sample heating, gather aldoketones material with 500ml/min DNPH pipe.After the effective 5ml acetonitrile of DNPH, analyze aldoketones content of material with high performance liquid chromatograph.
Test result is
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.100 |
| Acetone | 0.100 | 0.302 |
| Acrolein | 0.100 | Do not detect |
Embodiment 2
A preparation method for low VOC release bamboo fibre, comprises the following steps successively:
1), by bamboo fibre rinsing in water, be then dried to constant weight, baking temperature is 110 DEG C;
2), by neopelex be added to the water, be configured to the aqueous solution that concentration is 5g/L, continue stirring until neopelex and dissolve completely;
3), under Keep agitation, to step 2) add the toluene di-isocyanate(TDI) that methyl ethyl ketoxime closes end group in gained solution, the toluene di-isocyanate(TDI) addition that methyl ethyl ketoxime closes end group is 2% of aqueous solution quality, stir 10 minutes under 1000 revs/min of mixing speeds, obtain emulsion, be designated as modifier;
4), by bamboo fibre and step 3) gained modifier, and continue immersion 30 minutes, then sieving leaches bamboo fibre, and is dried to constant weight at 80 DEG C by the bamboo fibre leached;
5), by step 4) gained bamboo fibre carries out the heat treatment of 1 hour at 160 DEG C of temperature, can obtain low VOC release bamboo fibre.
100g low VOC that Example 2 obtains release bamboo fibre is placed in 210 DEG C of baking ovens process 15 minutes, then by it in 23 ± 2 DEG C, 24h in 50 ± 5%RH environment.Sample is put into 10L sampler bag, be filled with 5L high pure nitrogen, 60 DEG C are heated 2h ± 2min in VOC samples storehouse.After sample heating, gather aldoketones material with 500ml/min DNPH pipe.After the effective 5ml acetonitrile of DNPH, analyze aldoketones content of material with high performance liquid chromatograph.
Test result is
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.240 |
| Acetone | 0.100 | 0.823 |
| Acrolein | 0.100 | Do not detect |
Embodiment 3
A preparation method for low VOC release bamboo fibre, comprises the following steps successively:
1), by bamboo fibre rinsing in water, be then dried to constant weight, baking temperature is 85 DEG C;
2), by OP-10 be added to the water, be configured to the aqueous solution that concentration is 50g/L, continue stirring until OP-10 and dissolve completely;
3), under Keep agitation, to step 2) add the methyl diphenylene diisocyanate that methyl ethyl ketoxime closes end group in gained solution, the methyl diphenylene diisocyanate addition that methyl ethyl ketoxime closes end group is 8% of aqueous solution quality, stir 30 minutes under 1000 revs/min of mixing speeds, obtain emulsion, be designated as modifier;
4), by bamboo fibre step 3 is immersed) gained modifier, and continue immersion 15 minutes, then sieving leaches bamboo fibre, and is dried to constant weight at 60 DEG C by the bamboo fibre leached;
5), by step 4) gained bamboo fibre carries out the heat treatment of 2 hours at 160 DEG C of temperature, can obtain low VOC release bamboo fibre.
100g low VOC that Example 2 obtains release bamboo fibre is placed in 210 DEG C of baking ovens process 15 minutes, then by it in 23 ± 2 DEG C, 24h in 50 ± 5%RH environment.Sample is put into 10L sampler bag, be filled with 5L high pure nitrogen, 60 DEG C are heated 2h ± 2min in VOC samples storehouse.After sample heating, gather aldoketones material with 500ml/min DNPH pipe.After the effective 5ml acetonitrile of DNPH, analyze aldoketones content of material with high performance liquid chromatograph.
Test result is
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.270 |
| Acetone | 0.100 | 0.720 |
| Acrolein | 0.100 | Do not detect |
Embodiment 4
By embodiment 1 step 3) in the methyl ethyl ketoxime hexamethylene diisocyanate addition of closing end group be that 5% of aqueous solution quality changes 2% into; All the other are with embodiment 1.
Acquired results is described in table 1 below
Table 1
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.200 |
| Acetone | 0.100 | 0.620 |
| Acrolein | 0.100 | Do not detect |
Embodiment 5
By embodiment 1 step 3) in the methyl ethyl ketoxime hexamethylene diisocyanate addition of closing end group be that 5% of aqueous solution quality changes 8% into; All the other are with embodiment 1.
Acquired results is described in table 3 below
Table 3
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.170 |
| Acetone | 0.100 | 0.634 |
| Acrolein | 0.100 | Do not detect |
Embodiment 6
By embodiment 1 step 3) in the methyl ethyl ketoxime hexamethylene diisocyanate addition of closing end group be that 5% of aqueous solution quality changes 4% into; All the other are with embodiment 1.
Acquired results is described in table 4 below
Table 4
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.130 |
| Acetone | 0.100 | 0.375 |
| Acrolein | 0.100 | Do not detect |
Embodiment 7
By embodiment 1 step 3) in the methyl ethyl ketoxime hexamethylene diisocyanate addition of closing end group be that 5% of aqueous solution quality changes 6% into; All the other are with embodiment 1.
Acquired results is described in table 3 below
Table 3
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | Do not detect |
| Acetaldehyde | 0.100 | 0.146 |
| Acetone | 0.100 | 0.405 |
| Acrolein | 0.100 | Do not detect |
Comparative example 1
Get the undressed bamboo fibre of 100g and be placed in 210 DEG C of baking ovens process 15 minutes, then by it in 23 ± 2 DEG C, 24h in 50 ± 5%RH environment.Sample is put into 10L sampler bag, be filled with 5L high pure nitrogen, 60 DEG C are heated 2h ± 2min in VOC samples storehouse.After sample heating, gather aldoketones material with 500ml/min DNPH pipe.After the effective 5ml acetonitrile of DNPH, analyze aldoketones content of material with high performance liquid chromatograph.
Test result is
| Object | Detection limit (μ g) | Amount of collected (μ g) |
| Formaldehyde | 0.100 | 0.130 |
| Acetaldehyde | 0.100 | 14.280 |
| Acetone | 0.100 | 2.100 |
| Acrolein | 0.100 | 0.152 |
Can be drawn by above-mentioned experimental result:
1) after isocyanate-modified, the aldehydes release of bamboo fibre has obvious reduction;
2) aliphatic isocyanates is adopted, namely comparatively to adopt the aldehydes of aromatic isocyanate-modified bamboo fibre to discharge as the aldehydes release of modifier gained bamboo fibre low for the methyl ethyl ketoxime hexamethylene diisocyanate of closing end group, this is because aliphatic isocyanates has flexible higher aliphatic chain, therefore, there is better permeability to bamboo fibre, thus better cross-linking effect can be ensured.
3) if blocked isocyanate content is too low in modifier, then blocked isocyanate is lower in the adsorbance on bamboo fibre surface, and thus in bamboo fibre, hydroxy-containing component cannot fully be reacted, thus affects cross-linking effect; If its too high levels, then isocyanate groups cannot fully be reacted, thus affects cross-linking effect; Therefore, in modifier, blocked isocyanate consumption must remain in preferable range, can reach optimum cross-linking effect.
Finally, it is also to be noted that what enumerate above is only several specific embodiment of the present invention and comparative example.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (5)
1. a preparation method for low VOC release bamboo fibre, it is characterized in that, described preparation method comprises the following steps successively:
1), by bamboo fibre rinsing in water, be then dried to constant weight, baking temperature is 60 DEG C-110 DEG C;
2), by surfactant be added to the water, be configured to the aqueous solution that concentration is 5g/L-50g/L, continue stirring until surfactant and dissolve completely;
3), under Keep agitation, to step 2) add enclosed type isocyanic acid in obtained aqueous solution, blocked isocyanate addition is step 2) 2%-8% of described aqueous solution quality, stir 10 minutes-30 minutes under 800-1200 rev/min of mixing speed, obtain emulsion, be designated as modifier;
4), by bamboo fibre step 3 is immersed) gained modifier, and continue immersion 5 ~ 30 minutes, then sieving leaches bamboo fibre, and is dried to constant weight at 60 DEG C-80 DEG C by the bamboo fibre leached;
5), by step 4) gained bamboo fibre carries out the heat treatment of 30 minutes-120 minutes at 120 DEG C of-180 DEG C of temperature, can obtain low VOC release bamboo fibre.
2. the preparation method of low VOC release bamboo fibre according to claim 1 and 2, it is characterized in that, described step 2) in, surfactant is the mixture of any one or any two kinds in dodecyl phenenyl sulfate, lauryl sodium sulfate, OP-10, polysorbas20.
3. the preparation method of low VOC release bamboo fibre according to claim 1 and 2, it is characterized in that, described step 3) in, blocked isocyanate is adopt sodium hydrogensulfite, methyl ethyl ketoxime, acetylacetone,2,4-pentanedione, any one enclosed type hexamethylene diisocyanate (HDI) as sealer gained in epsilon-caprolactams or toluene di-isocyanate(TDI) (TDI) or methyl diphenylene diisocyanate (MDI).
4. the preparation method of low VOC release bamboo fibre according to claim 3, it is characterized in that, described blocked isocyanate is preferably the hexamethylene diisocyanate that methyl ethyl ketoxime closes end group.
5. the preparation method of the low VOC release bamboo fibre according to claim 1 or 4, is characterized in that, described step 3) in, preferred blocked isocyanate addition is step 2) 4%-6% of described aqueous solution quality.
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| CN109830335A (en) * | 2019-03-29 | 2019-05-31 | 安徽徽宁电器仪表集团有限公司 | A kind of tensile type shielded cable |
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| CN103210011A (en) * | 2010-09-23 | 2013-07-17 | 赢创德固赛有限公司 | Method for producing storage-stable polyurethane prepregs and molding bodies produced therefrom on the basis of a polyurethane composition in solution |
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| CN104690979A (en) * | 2015-02-16 | 2015-06-10 | 长春博超汽车零部件股份有限公司 | Low-VOC natural fiber composite as well as preparation method and application of composite |
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