CN102941605B - Special wood modifier and preparation method thereof - Google Patents
Special wood modifier and preparation method thereof Download PDFInfo
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- CN102941605B CN102941605B CN201210410647.2A CN201210410647A CN102941605B CN 102941605 B CN102941605 B CN 102941605B CN 201210410647 A CN201210410647 A CN 201210410647A CN 102941605 B CN102941605 B CN 102941605B
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Abstract
The invention discloses a kind of Special wood modifier and preparation method thereof, component containing following weight part: 500 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 400 parts, organosilicon 150 ~ 300 parts, basic catalyst 5 ~ 30 parts, auxiliary agent 10 ~ 50 parts, wherein said formaldehyde to be mass concentration be 35% ~ 37% the aqueous solution.Special wood modifier of the present invention is primarily of the low-molecular-weight modified phenolic resins composition of one, be characterized in that viscosity is low, good water solubility, stability in storage are good, synthesis technique is simple, burst size of methanal is low, be applicable to the modification of various seeds, especially to the modification of fast growing wood, economic worth is higher.And after processing timber with this properties-correcting agent, the density of base material, dimensional stability, hardness, water resisting property, erosion resistance are all greatly improved.
Description
Technical field
The present invention relates to a kind of properties-correcting agent, particularly relate to a kind of properties-correcting agent for Wooden modifying and preparation method thereof.
Technical background
Timber be society generally acknowledge four large building materials in unique reproducible building resource, it almost appears in all trades and professions.Dwell tree and breath to drilling wood to make fire from the ape man of ancient times, then to modern household operation, the mankind never left timber, can say that the development of the mankind is also carried out along with timber.
Along with the development of human civilization, it is the figure that the various industry of paper-making industry, upholstery, packing business, automobile industry etc. all be unable to do without woodwork.The consumption of timber is increasing, and China also becomes an importation of timber big country by a forest reserves big country, and domestic timber demand breach increases day by day.In order to alleviate this imbalance between supply and demand, country proposes the plan that fast-growing, high-yield woods is built, but along with the increase of fast-growing, high-yield woods area, domestic timber breach should reduce, but be through investigation find effect not picture anticipation so gather effect, the material of tracing it to its cause mainly because of fastgrowing trees is undesirable, easily deforms, density is low, and hardness is not high, only can be used in some and lower industry is required to material.So only have, fast growing wood is optimized, improves its performance, a current supply and demand difficult problem could be alleviated like this.
Timber optimization has the history of several thousand, and before can tracing back to 5200 the earliest, the Sa rice clansman in Northern Europe just causes by thermal treatment the dimensional stability that wood internal chemical reaction improves timber.And some part of stool of B.C. 2500 to 3000 of being unearthed from Egypt is just through chemical treatment, the Egyptian mural painting of B.C. 1900 be unearthed just shows that the timber of bow and crossbow is carried out chemical treatment by people at that time.Craftsman is also by the timber of chemical process process shipbuilding for the capital shipbuilding of eleventh century dimension, improves its water resisting property and dimensional stability.Timber is optimized long-standing thus, perhaps many treatment process are lost, but find that current optimization timber mainly contains two kinds of methods by By consulting literatures: one is by physical method process, such as by timber high temperature cabonization, by changing wood internal composition to improve its dimensional stability, or by wood compression, by improving density of wood substance to improve its stability; Two is by chemical modification process, such as, close the hydroxyl in timber to improve its stability with chemical feedstocks, or suppress its dimensional change to filled high polymer material in timber.Along with the development of science and technology, many experts find by advanced instrument research, cause the yielding major cause of timber to be because timber belongs to porous material.There is a large amount of capillary canals in inside, has extremely strong capillary force to glassware for drinking water, and wood cell wall exists again a large amount of pars amorphas be made up of hemicellulose and crystallizing field.All there is polarity group exposed in a large number in these regions---and mainly hydroxyl, when entering wood internal under the magnetism effect of water at kapillary, large quantity of moisture causes wood cell generation deformation with hydroxy combining, thus causes the change of wood dimensional stability.So the problem wanting to solve wood dimensional stability mainly still gives timber certain water resisting property, the material of some rigidity then will be filled with in timber by the hardness solving timber, so the key solving fast growing wood is exactly that the material some existing rigidity can being given again timber water resisting property is filled with in timber, only in this way, the use range of fast growing wood could expand.
Summary of the invention
The object of this invention is to provide a kind of moderate, technique is simple, burst size of methanal is low, the obvious timber properties-correcting agent of modified effect and preparation method thereof.
In order to achieve the above object, a kind of Special wood modifier of the present invention, component containing following weight part: 500 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 400 parts, organosilicon 150 ~ 300 parts, basic catalyst 5 ~ 30 parts, auxiliary agent 10 ~ 50 parts, wherein said formaldehyde to be mass concentration be 35% ~ 37% formalin.
Be preferably 600 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 300 parts, organosilicon 200 ~ 300 parts, basic catalyst 10 ~ 20 parts, auxiliary agent 20 ~ 30 parts, wherein said formaldehyde to be mass concentration be 35% ~ 37% formalin;
Be more preferably 720 parts, formaldehyde, 20 parts, urea, phenolic compound 250 parts, organosilicon 200 parts, basic catalyst 15 parts, auxiliary agent 20 parts, wherein said formaldehyde to be mass concentration be 35% ~ 37% formalin.
Phenolic compound of the present invention is selected from phenol, alkylphenol or aromatic base phenol, is preferably phenol, methylphenol, xylenol, methylolphenol, dihydroxyphenyl propane, is more preferably phenol, to xylenol, methylolphenol.
Silicoorganic compound of the present invention are selected from tetraethoxy, alkylsilanol, terminal hydroxy group siloxanes, phenyl alkoxysilane, dimethicone, methyltrimethoxy silane, be preferably alkylsilanol, terminal hydroxy group siloxanes, dimethicone, be more preferably methylol siloxanes, methyl silanol, ethyl silanol, propyl group silanol, hexamethyl cyclotrisiloxane, methyl-silicone oil.
Basic catalyst of the present invention can be the basic catalyst that any this area is commonly used, be preferably selected from sodium hydroxide, potassium hydroxide, hydrated barta, ammonium hydroxide, calcium hydroxide, quadrol, diethylamine, be more preferably sodium hydroxide, potassium hydroxide, hydrated barta, calcium hydroxide.
Auxiliary agent of the present invention is selected from sodium-chlor, Repone K, ammonium chloride, magnesium chloride, bariumchloride, aluminum chloride, is preferably Repone K, ammonium chloride, bariumchloride, aluminum chloride, more elects bariumchloride, aluminum chloride as.
The invention still further relates to the preparation method of above-mentioned Special wood modifier, its synthesis technique is as follows: join in reactor by the phenolic compound of thawing, start stirring, add the formaldehyde of 1/3 weight again, slowly add the basic catalyst of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, remaining formaldehyde and organosilicon is added after insulation terminates, and slowly add remaining basic catalyst, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, urea and auxiliary agent is added after insulation terminates, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid.
Special wood modifier of the present invention, the wherein selection of each component and each components by weight, be through the preferred range value that By consulting literatures and test of long duration draw.First be synthesis one methylolphenol and hydroxymethyl-phenol in properties-correcting agent preparation process, and then aggregate into micromolecular methylol prepolymer, and then under catalyst action, organosilicon is incorporated on phenol ring.Suppress organosilyl strong perviousness and leachability, improve rate of utilization and the effect weather resistance of raw material.When after properties-correcting agent solidification, phenolic compound can form support effect in the pars amorpha of wood cell wall as phenol, suppresses it to deform.The capillary wall of simultaneously outside also can cover one deck cured film, and organosilyl organic end can be evenly distributed in kapillary, form one deck hydrophobic membrane, suppress kapillary to the adsorption of water, and the phenol after solidification be three dimensional structure, organosilicon end is interspersed wherein, silicone hydroxyl under certain condition with the hydroxyl generation dehydration reaction on Mierocrystalline cellulose and hemicellulose, decrease the water suction group in timber, improve the water resisting property of timber.Moreover in insoluble rigid structure after phenolic glue solidification, both improve density of wood and turn increased hardness.
The feature of Special wood modifier of the present invention is that viscosity is low, good water solubility, stability in storage are good, synthesis technique is simple, burst size of methanal is low, and be applicable to the modification of various seeds, especially to the modification of fast growing wood, economic worth is higher.And after processing timber with this properties-correcting agent, the density of base material, dimensional stability, hardness, water resisting property, erosion resistance are all greatly improved.
Embodiment
Below in conjunction with embodiment and testing data, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
Embodiment 1
The feed composition of the following weight of precise:
Mass concentration is formalin 720 parts, 20 parts, urea, phenol 250 parts, methyl silanol 200 parts, 15 parts, sodium hydroxide, the bariumchloride 20 parts of 35%.
The phenol of thawing is joined in reactor, start stirring, add the formalin of 1/3 weight again, slowly add the basic catalyst sodium hydroxide of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, organosilicon and remaining formaldehyde solution is added after insulation terminates, and slowly add remaining basic catalyst, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, add urea and auxiliary agent, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid, be Wood modifier of the present invention.
Embodiment 2
The feed composition of the following weight of precise:
Mass concentration is formalin 350 parts, 10 parts, urea, xylenol 130 parts, methyl silanol 110 parts, hydrated barta 10 parts, the bariumchloride 10 parts of 36%.
The phenol of thawing is joined in reactor, start stirring, add the formalin of 1/3 weight again, slowly add the basic catalyst hydrated barta of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, remaining formaldehyde solution and organosilicon is added after insulation terminates, and slowly add remaining basic catalyst, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, add urea and auxiliary agent, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid, be Wood modifier of the present invention.
Embodiment 3
The feed composition of the following weight of precise:
Mass concentration is formalin 540 parts, 20 parts, urea, phenol 200 parts, ethyl silanol 165 parts, 15 parts, sodium hydroxide, 15 parts, the aluminum chloride of 36%.
The phenol of thawing is joined in reactor, start stirring, add the formalin of 1/3 weight again, slowly add the basic catalyst of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, remaining formaldehyde solution and organosilicon is added after insulation terminates, and slowly add remaining basic catalyst sodium hydroxide, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, add urea and auxiliary agent, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid, be Wood modifier of the present invention.
Embodiment 4
The feed composition of the following weight of precise:
Mass concentration is formalin 720 parts, 20 parts, urea, methylolphenol 250 parts, methyl silanol 200 parts, 20 parts, calcium hydroxide, the bariumchloride 20 parts of 35%.
The phenol of thawing is joined in reactor, start stirring, add the formalin of 1/3 weight again, slowly add the basic catalyst calcium hydroxide of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, remaining formaldehyde solution and organosilicon is added after insulation terminates, and slowly add remaining basic catalyst, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, add urea and auxiliary agent, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid, be Wood modifier of the present invention.
Embodiment 5
The feed composition of the following weight of precise:
Mass concentration is formalin 400 parts, 10 parts, urea, phenol 150 parts, methyl silanol 130 parts, 13 parts, potassium hydroxide, 15 parts, the aluminum chloride of 35%.
The phenol of thawing is joined in reactor, start stirring, add the formalin of 1/3 weight again, slowly add the basic catalyst potassium hydroxide of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, remaining formaldehyde solution and organosilicon is added after insulation terminates, and slowly add remaining basic catalyst, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, add urea and auxiliary agent, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid, be Wood modifier of the present invention.
Wood modifier of the present invention, prove through a large amount of tests, in other specific embodiments, the component of properties-correcting agent is at 500 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 400 parts, organosilicon 150 ~ 300 parts, basic catalyst 5 ~ 30 parts, all can reach desired effects within the scope of auxiliary agent 10 ~ 50 parts, density, hardness, dimensional stability, water resisting property all have greatly improved.When 600 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 300 parts, organosilicon 200 ~ 300 parts, basic catalyst 10 ~ 20 parts, during auxiliary agent 20 ~ 30 parts, modified effect is better.Preferably, wherein phenolic compound can be selected from phenol, to xylenol, methylolphenol; Silicoorganic compound can be selected from methylol siloxanes, methyl silanol, ethyl silanol, propyl group silanol, hexamethyl cyclotrisiloxane, methyl-silicone oil; Basic catalyst selected from sodium hydroxide, potassium hydroxide, hydrated barta, calcium hydroxide; Auxiliary agent can be selected from aluminum chloride or bariumchloride.Effect assessment
Special wood modifier of the present invention is to the test of the dimensional stability of timber, hardness and Effects of Density
The properties-correcting agent 500g that properties-correcting agent: test example 1-5 obtains and 65g water mix, and to obtain final product.
Method of modifying: adopt the modification of normal-temperature vacuum pressurization, pressurize 20min under vacuum tightness-0.095MPa, after under 0.6MPa condition, pressurize 1.5 hours.
Test specimen is dry: 45 DEG C are dried to water ratio and are less than 50%, and 55 DEG C are dried to water ratio and are less than 30%, and 65 DEG C are dried to water ratio and are less than 20%, and 80 DEG C are dried to water ratio and are less than 15%, and 120 DEG C are dried to water ratio and are less than 8%, and drying completes.
Test specimen base material: poplar (being provided with two kinds: process material and untreated material)
Specimen size: hardness determination specimen size: 100mm*50mm*20mm
Dimensional stability specimen size: 20mm*20mm*20mm
Test set: electronic type universal trier (model: WDW-10 Jinan monarch's billows ensaying experimental installation company limited)
Detection method: 1, hardness determination polarity formula universal testing machine detects specimen hardness, each survey is averaged for twice.
2, dimensional stability, water resisting property detect: detect the absolute dry mass before and after test specimen process, over dry volume before treatment, soak the volume after (40 DEG C of 72h) aftertreatment and quality
3, burst size of methanal detects and adopts perforation method to detect
Method of calculation: volume expansivity S=(V2-V1)/V1*100%
Nonshrink coefficient ASE=(S1-S2)/S1*100%
Rate of body weight gain WPG=(G2-G1)/G1*100%
Water-intake rate W1=(the G3-G1)/G1*100% of untreated material
Water-intake rate W2=(the G4-G2)/G2 of process material
Water absorption resistance RWA=(W1-W2)/W1
Density P=G/V
In formula: V1: the over dry volume of sample before immersion, mm
3;
V2: the over dry volume of sample before immersion, mm
3;
S1: the volume expansivity of untreated material;
S2: the volume expansivity of process material;
G1: untreated material over dry weight, g;
G2: process material over dry weight, g;
G3: the weight in wet base of untreated material, g:
G4: process weight in wet base, g;
W1: the water-intake rate of untreated material;
W2: the water-intake rate of process material.
Measuring result is as shown in table 1 to table 5:
Table 1 properties-correcting agent of the present invention is on the impact of wood dimensional stability
Table 2 properties-correcting agent of the present invention is on the impact of the hardness of wood
| Test number | Average hardness/KN | Changes in hardness rate |
| Experiment one | 3852.6 | 85.81% |
| Experiment two | 4213.21 | 103.20% |
| Experiment three | 4203.01 | 102.71% |
| Experiment four | 3953.7 | 90.69% |
| Experiment five | 4135.2 | 99.44% |
| Untreated material | 2073.4 |
Table 3 properties-correcting agent of the present invention is on the impact of density of wood
| Experiment numbers | Before process/g/m 3 | After process/g/m 3 | Increase rate |
| Experiment one | 0.3571 | 0.5632 | 57.71% |
| Experiment two | 0.3592 | 0.6302 | 75.45% |
| Experiment three | 0.3874 | 0.5843 | 50.83% |
| Experiment four | 0.3659 | 0.5921 | 61.82% |
| Experiment five | 0.3838 | 0.6135 | 59.85% |
Table 4 properties-correcting agent of the present invention is on the impact of timber water resisting property
| Experiment numbers | Absolutely dry quality/g | Complete wet quality/g | Water-intake rate | Anti-water-intake rate |
| Experiment one | 5.01 | 5.76 | 15% | 92.79% |
| Experiment two | 4.87 | 5.80 | 19% | 90.87% |
| Experiment three | 4.83 | 5.84 | 21% | 89.90% |
| Experiment four | 4.26 | 4.94 | 16% | 92.31% |
| Experiment five | 4.24 | 5.00 | 18% | 91.35% |
| Untreated material | 3.16 | 9.73 | 208% | 0 |
The burst size of methanal of timber after table 5 modifier modification of the present invention
| Experiment numbers | Burst size of methanal/mg/100g |
| Experiment one | 3.68 |
| Experiment two | 3.72 |
| Experiment three | 4.13 |
| Experiment four | 3.78 |
| Experiment five | 2.53 |
As can be seen from data in table 1-table 5: test specimen is after modifier treatment, and volume expansivity is down to about 3% by original 12.08%, reduces 75%; Nonshrink coefficient has brought up to about 75% by 0; Hardness improves about 80%; Density improves about 55%, anti-water-intake rate also brings up to about 90% by 0, these data are enough to show that the shortcoming of this properties-correcting agent to the dimensional stability of material, hardness, density aspect all has greatly improved, and burst size of methanal remains essentially between 2.5 ~ 4.5, meets environmental requirement completely.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (3)
1. a Special wood modifier, it is characterized in that, component containing following weight part: 500 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 400 parts, organosilicon 150 ~ 300 parts, basic catalyst 5 ~ 30 parts, auxiliary agent 10 ~ 50 parts, wherein said formaldehyde to be mass concentration be 35% ~ 37% the aqueous solution;
Described auxiliary agent be selected from sodium-chlor, Repone K, ammonium chloride, magnesium chloride, bariumchloride, aluminum chloride one or more;
Described phenolic compound be selected from phenol, methylphenol, xylenol, methylolphenol, dihydroxyphenyl propane one or more;
Silicoorganic compound be selected from tetraethoxy, alkylsilanol, terminal hydroxy group siloxanes, phenyl alkoxysilane, dimethicone, methyltrimethoxy silane one or more;
Synthesize as follows: the phenolic compound of thawing is joined in reactor, start stirring, add the formaldehyde solution of 1/3 weight again, slowly add the basic catalyst of 1/2 weight simultaneously, then heating is stopped by after still temperature rise to 45 DEG C ~ 50 DEG C, now still temperature continues to rise, control still temperature and be no more than 60 DEG C, at 50 DEG C of insulation 1h after intensification terminates, organosilicon and remaining formaldehyde solution is added after insulation terminates, and slowly add remaining basic catalyst, then by still temperature rise to 85 DEG C ~ 90 DEG C, insulation 1h, add urea and auxiliary agent, insulated and stirred was cooled to 30 DEG C after 30 minutes, obtain reddish-brown thick liquid, obtain.
2. Special wood modifier according to claim 1, it is characterized in that, component containing following weight part: 600 ~ 800 parts, formaldehyde, 20 parts, urea, phenolic compound 200 ~ 300 parts, organosilicon 200 ~ 300 parts, basic catalyst 10 ~ 20 parts, auxiliary agent 20 ~ 30 parts, wherein said formaldehyde to be mass concentration be 35% ~ 37% the aqueous solution.
3., according to the properties-correcting agent described in right 1 or 2, it is characterized in that, described basic catalyst be selected from sodium hydroxide, potassium hydroxide, hydrated barta, ammonium hydroxide, calcium hydroxide, quadrol, diethylamine one or more.
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| CN103145937B (en) * | 2013-03-19 | 2015-05-27 | 上海宝田新型建材有限公司 | Method for preparing hydroxyl-blocked polysiloxane-toughened modified phenolic resin |
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| CN107803902A (en) * | 2017-11-07 | 2018-03-16 | 桂林奥尼斯特节能环保科技有限责任公司 | A kind of dedicated modified liquid of timber and preparation method thereof |
| CN107877645A (en) * | 2017-11-07 | 2018-04-06 | 桂林奥尼斯特节能环保科技有限责任公司 | A kind of wood mould modification liquid and preparation method thereof |
| CN111308057B (en) * | 2019-11-04 | 2022-02-15 | 内蒙古农业大学 | Method for determining wood section processing conditions for veneer cutting and evaluating processing effect |
| CN113829454A (en) * | 2021-10-18 | 2021-12-24 | 福建省碧诚工贸有限公司 | Processing technology of anti-corrosion and anti-mildew plate |
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