CN104044193A - Resin type silicate wood modifier and preparation method of modified material of modifier - Google Patents
Resin type silicate wood modifier and preparation method of modified material of modifier Download PDFInfo
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Abstract
The invention belongs to a resin type silicate wood modifier and a preparation method of a modified material of the modifier. According to the preparation method, the resin type silicate wood modifier is prepared by taking melamine, formaldehyde, urea and soluble sodium silicate as main raw materials as well as respectively taking polyvinyl alcohol and diethylene glycol as a toughening agent and a stabilizer; the resin type silicate wood modifier can be stably stored for a long time and can be repeatedly recycled. The modifier has the advantages that the dimensional stability, the density, the surface hardness, the anti-bending strength, the anti-bending elastic modulus, the impact toughness and the wear resistance of artificial forest wood processed by virtue of the modifier are substantially improved, the modifier has the advantages that the flame retardance and environment-friendly effect are achieved, no pollution is caused to a human body and the environment, the leachability resistance of the modifier in the processed wood is improved, and the application value of the artificial forest wood is improved.
Description
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Technical field
The invention belongs to the preparation method of a kind of resin type silicate Wood modifier and modification material thereof.
Background technology
For many years, China artificial forest resource area surely occupies first place in the world always.Yet because artificial forest wood growth cycle is short, variability is large, often material is soft, density is little, intensity low (as poplar, China fir etc.), and its range of application is very limited, and added value of product is low.Adopting water-soluble low molecular weight melamine resin solution impregnation to process timber, can significantly improve the physical and mechanical properties such as its density, dimensional stability, bending strength and elastic modelling quantity, is a kind of effective method for modifying wood.Yet, this modifier also existence and stability poor, be difficult to long term storage, reduce timber toughness, function is relatively single, the more high defect of cost or problem, so be unfavorable for promoting.Water-soluble metasilicate solution is lower more than 1 times than the cost of this resin modified liquid, except improving hardness and the wearability of timber, also can give the anti-flaming function that timber is good.But this inorganic salt modification agent moisture absorption, not water-fast, causes processing material size unstable, and modifier easily runs off.If organic water dissolubility resin and inorganic silicate are combined, add organic alcohols material simultaneously, improve its stability and toughness, both have complementary advantages, form a kind of can long term storage and the low-cost multi-functional timber modifier of recycling, be expected to substitute function singleness in Vehicles Collected from Market, modification liquid that cost is higher, physical and mechanical property and the fire resistance of comprehensive change artificial forest wood, to realizing, the increment of artificial forest wood efficiently utilizes and the sustainable development of China's Forest Resources is significant.
Summary of the invention
The object of the invention is to design the preparation method of a kind of resin type silicate Wood modifier and modification material thereof, can make to be largely increased through dimensional stability, density, case hardness, bending strength, Deflection Modulus of Elasticity, impact flexibility and the wearability of the artificial forest wood of this modifier treatment, there is anti-flaming function simultaneously, and environmental protection, nuisanceless to human body and environment, after processing, in timber, the resistance leachability of modifier is also enhanced, and has improved the advantage of the using value of artificial forest wood.
For this reason, the preparation method of resin type silicate Wood modifier of the present invention and modification material thereof, step is as follows:
(1) proportioning that is 1:2 ~ 3:0.2 ~ 1.0 according to melamine, formaldehyde, urea mol ratio is got the raw materials ready, mensuration dissolubility silicic sodium solution addition is melamine 20% ~ 50%, polyvinyl alcohol and diethylene glycol (DEG) addition are respectively 0.1% ~ 5% and 10% ~ 30% of formaldehyde, catalyst is NaOH and acetic acid solution, mass percent concentration is respectively 20% and 10%, and the mass percent concentration of formaldehyde and sodium silicate solution is respectively 37% and 30%;
(2) formaldehyde and polyvinyl alcohol being added in reactor, be warming up to 50 ~ 60 ℃, is 4.0 ~ 5.0 by acetic acid regulator solution pH value after stirring, and temperature remains on 60～70 ℃, reacts 10～30 minutes, obtains the mixed liquor of formaldehyde and polyvinyl formal;
(3) with NaOH, regulating this pH of mixed value is 8.0 ~ 9.0, add melamine and diethylene glycol (DEG), temperature remains on 70～80 ℃, reacts 40～60 minutes, obtains the mixed liquor of formaldehyde, polyvinyl formal and the melamine resin after diethylene glycol (DEG) etherificate;
(4) mixeding liquid temperature of melamine resin is reduced to 60～70 ℃, adds urea, react 10～20 minutes, obtain the mixed liquor of polyvinyl formal and the melamine resin after diethylene glycol (DEG) etherificate and a small amount of Lauxite.
(5) mixeding liquid temperature of melamine resin and a small amount of Lauxite is reduced to 50～60 ℃, add mensuration dissolubility silicic sodium solution, continue reaction, when the mixing multiple and be 1:3～10 of this reactant liquor and water, reduce below temperature to 40 ℃, and to regulate this reacting liquid pH value with NaOH be 9.5 ~ 10.5, obtain resin type silicate solutions;
(6) by moisture content, be 10% or following artificial forest wood put into airtight impregnation process tank, vacuumizing and making negative pressure in tank is-0.1～-0.08MPa, keeps 30～60 minutes;
(7) synthetic resin type silicate solutions is added after water, making its solid containing is 15%～30%, utilize the suction function in impregnation process tank that resin type silicate solutions is flooded to timber completely and injects timber, remove vacuum, air pressure to applying 0.6～-2.0MPa in tank body, keeps 1～4 hour.
(8) pressure relief, remaining resin type silicate solutions is discharged, stores, reused, processing material is shifted out outside tank, gas is done to after moisture content is below 50%, moving to dry kiln dries, 40～80 ℃ of baking temperatures, 7～20 days drying times, finally obtain moisture content and are 5%～8% modification material.
Described artificial forest wood is poplar, willow, China fir, cryptomeria wood.
Said method has reached object of the present invention.
The present invention can make to be largely increased through the dimensional stability of the artificial forest wood of this modifier treatment, density, case hardness, bending strength, Deflection Modulus of Elasticity, impact flexibility and wearability, there is anti-flaming function simultaneously, and environmental protection, nuisanceless to human body and environment, after processing, in timber, the resistance leachability of modifier is also enhanced, and has improved the advantage of the using value of artificial forest wood.
The present invention is with melamine, formaldehyde, urea and soluble glass are primary raw material, with polyvinyl alcohol and diethylene glycol (DEG), be respectively flexibilizer and stabilizing agent, prepare a kind of resin type silicate Wood modifier, by vacuum pressed impregnation process, make artificial forest poplar, the dimensional stability of the timber such as China fir, density, case hardness, bending strength, Deflection Modulus of Elasticity, impact flexibility and wearability are largely increased, give the anti-flaming function that timber is good simultaneously, and environmental protection, nuisanceless to human body and environment, after processing, in timber, the resistance leachability of modifier is also enhanced, make to process material and can be widely used in floor, door and window, wallboard, the processing of the products such as furniture, greatly widened the range of application of artificial forest wood, really realized the excellent use of bad material.And this modifier can longer-term, stably store, realize repetitive cycling utilization.
The specific embodiment
A preparation method for resin type silicate Wood modifier and modification material thereof, step is as follows;
(proportioning that (1) is 1:2 ~ 3:0.2 ~ 1.0 according to melamine, formaldehyde, urea mol ratio is got the raw materials ready, mensuration dissolubility silicic sodium solution addition is melamine 20% ~ 50%, polyvinyl alcohol and diethylene glycol (DEG) addition are respectively 0.1% ~ 5% and 10% ~ 30% of formaldehyde, catalyst is NaOH and acetic acid solution, mass percent concentration is respectively 20% and 10%, and the mass percent concentration of formaldehyde and sodium silicate solution is respectively 37% and 30%;
(2) formaldehyde and polyvinyl alcohol being added in reactor, be warming up to 50 ~ 60 ℃, is 4.0 ~ 5.0 by acetic acid regulator solution pH value after stirring, and temperature remains on 60～70 ℃, reacts 10～30 minutes, obtains the mixed liquor of formaldehyde and polyvinyl formal;
(3) with NaOH, regulating this pH of mixed value is 8.0 ~ 9.0, add melamine and diethylene glycol (DEG), temperature remains on 70～80 ℃, reacts 40～60 minutes, obtains the mixed liquor of formaldehyde, polyvinyl formal and the melamine resin after diethylene glycol (DEG) etherificate;
(4) mixeding liquid temperature of melamine resin is reduced to 60～70 ℃, adds urea, react 10～20 minutes, obtain the mixed liquor of polyvinyl formal and the melamine resin after diethylene glycol (DEG) etherificate and a small amount of Lauxite.
(5) mixeding liquid temperature of melamine resin and a small amount of Lauxite is reduced to 50～60 ℃, add mensuration dissolubility silicic sodium solution, continue reaction, when the mixing multiple and be 1:3～10 of this reactant liquor and water, reduce below temperature to 40 ℃, and to regulate this reacting liquid pH value with NaOH be 9.5 ~ 10.5, obtain resin type silicate solutions;
(6) by moisture content, be 10% or following artificial forest wood put into airtight impregnation process tank, vacuumizing and making negative pressure in tank is-0.1～-0.08MPa, keeps 30～60 minutes;
(7) synthetic resin type silicate solutions is added after water, making its solid containing is 15%～30%, utilize the suction function in impregnation process tank that resin type silicate solutions is flooded to timber completely and injects timber, remove vacuum, air pressure to applying 0.6～-2.0MPa in tank body, keeps 1～4 hour.
(8) pressure relief, remaining resin type silicate solutions is discharged, stores, reused, processing material is shifted out outside tank, gas is done to after moisture content is below 50%, moving to dry kiln dries, 40～80 ℃ of baking temperatures, 7～20 days drying times, finally obtain moisture content and are 5%～8% modification material.
Described artificial forest wood is poplar, willow, China fir, cryptomeria wood.
A preparation method for resin type silicate Wood modifier, step is as follows:
The proportioning that is 1:2 ~ 3:0.2 ~ 1.0 according to melamine, formaldehyde, urea mol ratio is got the raw materials ready, mensuration dissolubility silicic sodium solution addition is melamine 20% ~ 50%, polyvinyl alcohol and diethylene glycol (DEG) addition are respectively 0.1% ~ 5% and 10% ~ 30% of formaldehyde, catalyst is NaOH and acetic acid solution, mass percent concentration is respectively 20% and 10%, and the mass percent concentration of formaldehyde and sodium silicate solution is respectively 37% and 30%.Formaldehyde and polyvinyl alcohol being added in reactor, be warming up to 50 ℃, is 5.0 by acetic acid regulator solution pH value after stirring, and temperature remains on 60 ℃, reacts 20 minutes.By sodium hydrate regulator solution pH value, be 9.0, add melamine and diethylene glycol (DEG), temperature remains on 75 ℃, reacts 60 minutes.Reduce temperature to 60 ℃, add urea, react 20 minutes.Reduce temperature to 50 ℃, add sodium silicate solution, continue reaction.When the mixing multiple and be 1:5 of reactant liquor and water, reduce temperature to 30 ℃, and be 10.0 with sodium hydrate regulator solution pH value, obtain resin type silicate and flood modification liquid.
The property indices of testing the silicate modified liquid of this resin type according to GB/T 14074-2006 < < based Wood Adhesives and resin method of inspection > > thereof is as follows:
Outward appearance: colourless uniform liquid;
Solids content: 54.6%;
PH value: 10.0;
Viscosity: 26～55 mPas;
Free formaldehyde content: 0.15%;
Water mixing multiple: 4～5 times;
Storage life: 30～60 days.
Outside the present invention, the artificial tree of reason detection data are as follows:
By specification be 2000mm * 200mm * 25mm(longitudinally * tangential * radially), the moisture content artificial forest cottonwood plank stuff that is 10% regular pile up in impregnation process tank body, and sheet material is fixed, close process tank, start to vacuumize, make the negative pressure state of reach-0.096MPa of tank interior, keep 45min; Synthetic dipping modification liquid is added after water, make it solid containing being 20%, utilize the suction function in impregnation process tank that modification liquid is injected and flood completely timber, remove vacuum, the air pressure to applying 0.8MPa in tank body, keeps 2 hours.Pressure relief, will remain modification liquid and discharge, and processings material is shifted out outside tank, and gas is done to after moisture content is 50% below, moves to dry kiln at the temperature of 40～80 ℃, is dried 10 days, obtains modifying cotton wood processing material.
Every physical and mechanical property index before and after modifying cotton wood being processed according to GB/T 1927 ~ 1943-2009 < < Physico-mechanical Properties of The Wood test method > > detects:
Timber rate of body weight gain 35% after processing, moisture content 6%, density is by the 0.37g/cm before processing
3increase to 0.65g/cm
3;
Anti-swollen rate can reach more than 50%;
Deflection Modulus of Elasticity increases to 13.5Gpa by 8.4Gpa;
Bending strength increases to 112.4Mpa by 58.5Mpa;
Case hardness increases to 3858.3 N by 1085.8 N;
Impact flexibility is by 30.13 KJ/m
2increase to 35.48 KJ/m
2;
Wearing valve is reduced to 54.6 mg/100r by 79.8 mg/100r, illustrates that wearability increases.
According to GB/T 2406.2-2009 < < plastics, with oxygen index method, measure burning behavior > > test modifying cotton wood and process the oxygen index (OI) of front and back, result is: oxygen index (OI) brings up to 52% by 24% before processing; Combustibility before and after processing according to the hot burst size-taper of ISO 5660-1:2002 < < calorimeter method of testing > > test modifying cotton wood, result is: HRR is by the 285.2kw/m before processing
2be reduced to 154.5kw/m
2, the total heat release of first 5 minutes is by 32.0MJ/m
2be reduced to 19.6 MJ/m
2, total smoke release is by 286.24m
2m
-2be reduced to 19.37m
2m
-2.Illustrate after modification, anti-flammability and the smoke-suppressing of poplar significantly improve.
The free formaldehyde content that discharges the > > test modifying cotton wood material of limiting the quantity of according to formaldehyde in GB18580-2001 < < indoor decorating and refurnishing materials, wood-based plate and goods thereof is 0.3mg/L, reaches Japanese F**** grade standard.
According to the standard method of test > > of U.S. AWPA E11-06 < < timber preservative leachability, measure the turnover rate of modifier in the timber of silicate modified dose of resin type and sodium silicate solution difference impregnation process, result is: the modifier turnover rate of the silicate modified material of resin type and sodium metasilicate modification material is respectively 1.3% and 7.5%, illustrate resin to silicate effectively retaining in timber play fixation, the resistance leachability that resin type is silicate modified dose is better, modification timeliness to timber is longer.
Adopt the artificial forest wood after resin type silicate Wood modifier impregnation process of the present invention, have that density is large, the advantage such as intensity and case hardness is high, dimensionally stable, abrasion resistant fire blocking, can be widely used in the products such as floor, door and window, wallboard, furniture, market prospects are wide.
In a word, the present invention can make to be largely increased through the dimensional stability of the artificial forest wood of this modifier treatment, density, case hardness, bending strength, Deflection Modulus of Elasticity, impact flexibility and wearability, there is anti-flaming function simultaneously, and environmental protection, nuisanceless to human body and environment, after processing, in timber, the resistance leachability of modifier is also enhanced, and has improved the advantage of the using value of artificial forest wood.
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Claims (2)
1. a preparation method for resin type silicate Wood modifier and modification material thereof, is characterized in that: step is as follows,
(1) proportioning that is 1:2 ~ 3:0.2 ~ 1.0 according to melamine, formaldehyde, urea mol ratio is got the raw materials ready, mensuration dissolubility silicic sodium solution addition is melamine 20% ~ 50%, polyvinyl alcohol and diethylene glycol (DEG) addition are respectively 0.1% ~ 5% and 10% ~ 30% of formaldehyde, catalyst is NaOH and acetic acid solution, mass percent concentration is respectively 20% and 10%, and the mass percent concentration of formaldehyde and sodium silicate solution is respectively 37% and 30%;
(2) formaldehyde and polyvinyl alcohol being added in reactor, be warming up to 50 ~ 60 ℃, is 4.0 ~ 5.0 by acetic acid regulator solution pH value after stirring, and temperature remains on 60～70 ℃, reacts 10～30 minutes, obtains the mixed liquor of formaldehyde and polyvinyl formal;
(3) with NaOH, regulating this pH of mixed value is 8.0 ~ 9.0, add melamine and diethylene glycol (DEG), temperature remains on 70～80 ℃, reacts 40～60 minutes, obtains the mixed liquor of formaldehyde, polyvinyl formal and the melamine resin after diethylene glycol (DEG) etherificate;
(4) mixeding liquid temperature of melamine resin is reduced to 60～70 ℃, adds urea, react 10～20 minutes, obtain the mixed liquor of polyvinyl formal and the melamine resin after diethylene glycol (DEG) etherificate and a small amount of Lauxite;
(5) mixeding liquid temperature of melamine resin and a small amount of Lauxite is reduced to 50～60 ℃, add mensuration dissolubility silicic sodium solution, continue reaction, when the mixing multiple and be 1:3～10 of this reactant liquor and water, reduce below temperature to 40 ℃, and to regulate this reacting liquid pH value with NaOH be 9.5 ~ 10.5, obtain resin type silicate solutions;
(6) by moisture content, be 10% or following artificial forest wood put into airtight impregnation process tank, vacuumizing and making negative pressure in tank is-0.1～-0.08MPa, keeps 30～60 minutes;
(7) synthetic resin type silicate solutions is added after water, making its solid containing is 15%～30%, utilize the suction function in impregnation process tank that resin type silicate solutions is flooded to timber completely and injects timber, remove vacuum, air pressure to applying 0.6～-2.0MPa in tank body, keeps 1～4 hour;
(8) pressure relief, remaining resin type silicate solutions is discharged, stores, reused, processing material is shifted out outside tank, gas is done to after moisture content is below 50%, moving to dry kiln dries, 40～80 ℃ of baking temperatures, 7～20 days drying times, finally obtain moisture content and are 5%～8% modification material.
2. by the preparation method of a kind of resin type silicate Wood modifier claimed in claim 1 and modification material thereof, it is characterized in that: described artificial forest wood is poplar willow, China fir, cryptomeria wood.
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| CN105500483A (en) * | 2015-12-01 | 2016-04-20 | 安徽雪峰木业有限公司 | Antifouling wood softening agent capable of improving handfeeling of woods and preparation method of antifouling wood softening agent |
| CN105563579A (en) * | 2015-12-23 | 2016-05-11 | 中国林业科学研究院木材工业研究所 | High-permeability resin type timber enhancing modifier and efficient immersion treatment control method |
| CN105583926A (en) * | 2014-10-21 | 2016-05-18 | 贾超 | Timber modification agent and preparation method thereof |
| CN107322741A (en) * | 2017-08-10 | 2017-11-07 | 马鞍山市谷庆门业有限公司 | A kind of China fir boarded door processing technology |
| CN114505935A (en) * | 2020-11-16 | 2022-05-17 | 深圳碳十四科技创新有限公司 | Preparation method of multifunctional micro-nano structure modified wood |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105583926A (en) * | 2014-10-21 | 2016-05-18 | 贾超 | Timber modification agent and preparation method thereof |
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| CN114505935A (en) * | 2020-11-16 | 2022-05-17 | 深圳碳十四科技创新有限公司 | Preparation method of multifunctional micro-nano structure modified wood |
| CN116214654A (en) * | 2023-02-08 | 2023-06-06 | 千年舟新材科技集团股份有限公司 | Fast-growing wood reinforcing process |
| CN116214654B (en) * | 2023-02-08 | 2024-03-29 | 千年舟新材科技集团股份有限公司 | Fast-growing wood reinforcing process |
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