CN107599093B - Water-borne functional wood modifier and treatment method thereof - Google Patents
Water-borne functional wood modifier and treatment method thereof Download PDFInfo
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Abstract
The invention relates to a water-borne functional wood modifier and a treatment method thereof, wherein the water-borne functional wood modifier comprises the following components, by weight, 100 parts of phenol, 100 ~ 150 parts of formaldehyde, 80 ~ 150 parts of dimethylol dihydroxy ethylene urea, 10 ~ 30 parts of dimethylol dihydroxy ethylene urea catalyst, 30 ~ 50 parts of silica sol, 25 ~ 35 parts of sodium hydroxide solution and 20 ~ 40 parts of hydrochloric acid solution.
Description
Technical Field
The invention relates to a water-borne functional wood modifier and a treatment method thereof, belonging to the technical field of wood processing.
Background
China is the second and the first world of large wood consumption, and the annual consumption is nearly 5 billion cubic meters (including logs, artificial boards and the like). According to the development report of Chinese forestry in 2015, the dependence of wood resource supply in China on the external environment reaches 50%, which exceeds the warning line, and along with the importance of environmental protection in various countries in the world, imported wood is less and less. The annual forest cutting limit during the period of 'thirteen five' of the country covered by the national institute of 3 months in 2016 is 25403.6 ten thousand cubic meters, which is reduced by nearly 7 percent compared with the period of 'twelve five'. Therefore, the contradiction between the effective supply of wood resources and the ever-increasing social demand in China is increasingly prominent. According to the eighth national forest resource clearing result, the area of the artificial forest in China is 0.69 hundred million hectares and is the first place in the world. Therefore, the artificial forest is vigorously developed, natural forest wood with seriously insufficient total amount in China and imported high-quality wood resources are replaced by artificial forest wood resources, and the method is an effective way for solving the problem of wood supply in China and realizing sustainable development of wood utilization. However, the artificial forest wood has the defects of low density, soft material, low strength, easy decay, flammability and the like, and the application of the artificial forest wood in the aspects of building materials, furniture manufacture and the like is limited, so that the functional improvement of the artificial forest wood is required for improving the quality grade of the artificial forest wood and realizing the value-added utilization of the artificial forest wood.
The wood modification is mainly to treat the wood by adopting a physical or chemical method or a method of using both the physical and chemical methods to improve the performance of the wood and endow the wood with new functions. The chemical modification is a main means for modifying the wood of the artificial forest, the resin-impregnated modified wood is a relatively successful industrialized wood modification method at present, but the impregnated modified wood selected from the common urea-formaldehyde resin, the phenolic resin, the furfuryl alcohol resin and the like has the problems of single functionalization of the modified wood, large molecular weight of a modified liquid medicine, environmental pollution, high comprehensive cost and the like. Therefore, research and development of a low-molecular-weight, low-free-formaldehyde-content and low-cost composite multifunctional wood modifying agent has become a research hotspot at present.
The phenolic resin has the characteristics of water resistance, weather resistance, wear resistance and the like, and has the advantages of better shrinkage resistance and aging resistance than urea-formaldehyde resin and less chemical agent loss in the drying process than furfuryl alcohol resin. In the technical field, the related patent technologies of the organic/inorganic composite wood modifier related to the phenolic resin are disclosed as follows:
patent CN201310421156.2 "a phenolic resin wood adhesive modifier and its application" discloses a phenolic resin modified adhesive for wood and bamboo impregnation, comprising: mixing the phenolic resin adhesive and a modifier (polyvinyl alcohol 17880-50 parts, silicon dioxide particles 1-12 parts, titanium dioxide particles 1-12 parts, polyvinylpyrrolidone K300.1-5 parts and a nonionic surfactant alkylphenol polyoxyethylene ether 0.1-1.5 parts) thereof according to a ratio of 1:1-8 to prepare the modifier. The medicament adopts phenolic resin adhesive as a main agent, and has the problems of large molecular weight and uniform permeation of a modifier.
Patent CN201510344965.7 "a nano-copper modified low molecular weight phenolic resin and its preparation method" discloses a method for preparing a nano-copper modified low molecular weight phenolic resin modifier for wood impregnation, wherein the main liquid medicine comprises phenol, copper sulfate mixed solution (copper sulfate, disodium ethylenediamine tetraacetate, polyvinylpyrrolidone, sodium hydroxide), formaldehyde mixed solution (formaldehyde aqueous solution, sodium pyrophosphate, potassium sodium tartrate) and sodium hydroxide aqueous solution. The method comprises the steps of in-situ synthesis of nano-copper while synthesizing water-soluble low-molecular-weight phenolic resin, pre-polymerization, in-situ synthesis of nano-copper and repolymerization. The mechanical property, the dimensional stability and the durability of the modified wood are improved, but the synthesis process is complex and the comprehensive cost is high.
Patent CN201410308703.0 "a preparation method and application of a multifunctional resin modifier for wood impregnation" uses phenol, formaldehyde, melamine, urea as main agents, boric acid and zinc borate as functional main agents, and a certain amount of dipropylene glycol is added to synthesize a low-alkaline multi-element copolycondensation resin modifier with weight gain enhancement, flame retardation and corrosion prevention functions;
patent CN201510001987.3 "preparation method and application method of modified phenolic resin suitable for improving flame retardant function of wood building material" one-time feeding phenol and formaldehyde as main agents, adding boric acid in the synthesis process, and preparing a modified phenolic resin medicament with excellent flame retardant function. Boron compounds have good flame retardancy, but such inorganic flame retardants are highly hygroscopic and easily lost.
Disclosure of Invention
The invention provides a water-borne functional wood modifier and a modification treatment method thereof, aiming at overcoming the research hotspot and the existing problems of the existing wood modifier, fully and uniformly permeating the artificial forest wood, obviously improving the dimensional stability and the physical mechanical property of the wood, endowing the wood with anticorrosion and flame retardant properties, low free formaldehyde content and environmental friendliness.
The technical scheme is that the water-borne functional wood modifier comprises, by weight, 100 parts of phenol, 100 ~ 150 parts of formaldehyde, 80 ~ 150 parts of dimethylol dihydroxy ethylene urea, 10 ~ 30 parts of dimethylol dihydroxy ethylene urea catalyst, 30 ~ 50 parts of silica sol, 25 ~ 35 parts of sodium hydroxide solution and 20 ~ 40 parts of hydrochloric acid solution.
The modifier is synthesized according to the following method:
adding phenol and 37 mass percent of formaldehyde solution into a reaction kettle, heating and stirring, controlling the temperature range to be 40 ~ 45 ℃, and adjusting the pH value of the solution to 9.0 ~ 10.0.0 by using 30 mass percent of sodium hydroxide solution;
secondly, because the reaction of the phenol and the formaldehyde is an exothermic reaction, the temperature of the mixed solution is quickly raised to 75 ~ 85 ℃, the reaction temperature is controlled and kept for 60 ~ 90 minutes;
regulating the pH of the mixed solution to 8.0 ~ 9.0.0 by using a hydrochloric acid solution with the concentration of 20%, cooling to 30 ~ 40 ℃, and continuously reacting for 20 ~ 30 minutes under the condition of stirring to obtain a hydroxymethyl phenol monomer solution;
adding 10-45% of dimethylol dihydroxy ethylene urea and silica sol into the prepared hydroxymethyl phenol monomer solution, mixing, and magnetically stirring for 10 ~ 20 minutes at room temperature;
fifthly, adding a dimethylol dihydroxy ethylene urea catalyst, adjusting the pH of the mixed solution to 7.5 ~ 8 by using a hydrochloric acid solution with the concentration of 20%, and magnetically stirring for 10 ~ 15 minutes until the solution is uniform to obtain the water-borne functional modifier.
A method for processing a water-borne functional modifier for artificial forest wood comprises the following steps:
firstly, diluting the prepared modifier with water, and adjusting the concentration to the required concentration for later use;
secondly, putting the artificial forest wood with the water content of 10 percent or less into a closed dipping treatment tank, vacuumizing to ensure that the negative pressure in the tank is-0.08 ~ -0.01MPa, and keeping for 45 ~ 60 minutes;
thirdly, injecting modifier liquid medicine into the treatment tank by utilizing the negative pressure effect in the dipping treatment tank, submerging the wood, relieving the vacuum, and carrying out progressive pressurization, wherein the pressurization is 0.1 ~ 0.2.2 MPa each time, the maintenance is carried out for 10 ~ 20 minutes, the process is repeated for 5 ~ 15 times until the air pressure of 0.8 ~ 1.5.5 MPa is applied, and the maintenance is carried out for 4 ~ 6 hours;
and fourthly, releasing the pressure of the impregnation treatment tank, discharging the residual modifier, taking out the impregnated wood, and drying the impregnated wood in a kiln until the water content is 8 ~ 12%.
The beneficial effect of the invention is that,
1) hydroxymethyl phenol active monomers mainly generated through the reaction of phenol and formaldehyde, such as mono-hydroxymethyl phenol, di-hydroxymethyl phenol and the like, are mixed with dimethylol dihydroxy ethylene urea and silica sol to form a stable sol system solution, and after wood is soaked, a polymer is formed by combining a heating and curing process with the cell wall and the cell cavity of the wood through covalent bonds, so that the synthetic process is simple and easy to operate;
2) the modifier has low molecular weight, is easy to uniformly permeate wood and has good treatment effect;
3) monomer active functional groups in the modifier are easy to react with hydroxyl of wood cell walls, so that the monomer active functional groups are fixed in the wood cell walls, the dimensional stability of the wood is obviously improved, and the modified artificial forest wood has the advantages of high density, high strength, corrosion resistance, flame retardance, good processability, environment-friendly production and the like;
4) the modified wood can be widely used for floors, solid wood doors and windows, furniture, interior decoration materials and the like, and can also be used for outdoor buildings such as wooden trestles, wayside pavilions and the like, so that the application range of the wood of the artificial forest is expanded.
Detailed Description
Example 1
The process method for synthesizing and preparing the water-borne functional wood modifier comprises the following steps:
adding 100 parts of phenol and 120 parts of formaldehyde solution with the mass percentage concentration of 37% into a reaction kettle, heating and stirring, controlling the reaction temperature to be 40 ℃, and adjusting the pH value to 9.0 by using NaOH solution with the concentration of 30%;
secondly, because the reaction of the phenol and the formaldehyde is an exothermic reaction, the temperature of the mixed solution is quickly raised to 75 ℃, the reaction temperature is controlled and kept for 70 minutes;
thirdly, regulating the pH value of the solution to 8.0 by using a hydrochloric acid solution with the concentration of 20 percent, cooling to 30 ℃, and continuously reacting for 25 minutes under the condition of stirring to obtain a hydroxymethyl phenol monomer solution;
adding 25% of dimethylol dihydroxy ethylene urea and silica sol into the prepared hydroxymethyl phenol monomer solution, mixing, and magnetically stirring for 20 minutes at room temperature;
fifthly, adding a dimethylol dihydroxy ethylene urea catalyst, adjusting the pH value of the solution to 7.5 by using a hydrochloric acid solution with the concentration of 20 percent, magnetically stirring for 15 minutes until the solution is uniform, and discharging.
The method for processing the artificial fir water-borne functional modifier comprises the following steps:
firstly, diluting the prepared modifier with water until the mass fraction of the modifier solution is 20 percent for later use;
secondly, filling the artificial Chinese fir with the water content of less than 10 percent in the specification size of 1000mm multiplied by 200mm multiplied by 25mm into a closed dipping treatment tank, vacuumizing to enable the negative pressure in the tank to be-0.09 MPa, and keeping for 45 minutes;
injecting the modifier liquid medicine into the treatment tank by utilizing the negative pressure effect in the impregnation treatment tank, submerging the wood, relieving the vacuum, carrying out progressive pressurization, pressurizing for 0.2MPa each time, keeping for 20 minutes, repeating for 6 times until the air pressure of 1.2MPa is applied, and keeping for 6 hours;
and fourthly, releasing the pressure of the impregnation treatment tank, discharging the residual modifier, taking out the impregnated wood, and drying in a kiln until the moisture content is 12% to obtain the modified wood.
The method is characterized in that various physical and mechanical property indexes before and after wood modification treatment are detected according to standard methods such as GB/T1927 ~ 1943-2009 test method for physical and mechanical properties of wood, and the results are that the weight gain rate of the treated wood reaches 34%, the water content is 10%, and the density is 0.348g/cm before treatment3Increased to 0.611g/cm3(ii) a The expansion resistance is improved by more than 56 percent; the bending elastic modulus is increased from 4.9GPa to 7.3 GPa; the bending strength is increased from 46.8MPa to 81.2 MPa; the surface hardness increased from 1014N to 2510N.
The formaldehyde emission of the modified cedarwood is tested according to a dryer method in GB 18580-2001 Formaldehyde emission limits in interior decoration materials, artificial boards and products thereof, and the test value is less than 0.45 mg/L.
According to GB/T2406.2-2009 'determination of combustion behavior by oxygen index method for plastics' test oxygen index before and after modification treatment of fir, the result is: the oxygen index increased from 23% to 43% before treatment.
According to GB/T13942.1-2009 durability of Wood, part 1: the natural corrosion resistance laboratory test method determines the corrosion resistance of the fir before and after treatment, and the result is as follows: the weight loss rates of the material and the treated fir modified material after being decayed by wood decay fungi are 65.9 percent and 10.5 percent respectively, which shows that the corrosion resistance of the modified fir is improved.
Example 2
The synthesis process for preparing the water-borne functional wood modifier comprises the following steps:
adding 100 parts of phenol and 130 parts of formaldehyde solution with the mass percentage concentration of 37% into a reaction kettle, heating and stirring, controlling the reaction temperature to be 40 ℃, and adjusting the pH value to 9.0 by using NaOH solution with the concentration of 30%;
secondly, because the reaction of the phenol and the formaldehyde is an exothermic reaction, the temperature of the mixed solution is quickly raised to 80 ℃, the reaction temperature is controlled and kept for 60 minutes;
thirdly, regulating the pH value of the solution to 8.0 by using hydrochloric acid with the concentration of 20 percent, cooling to 30 ℃, and continuously reacting for 30 minutes under the condition of stirring to obtain a hydroxymethyl phenol monomer solution;
adding 30 percent of dimethylol dihydroxy ethylene urea and silica sol into the prepared hydroxymethyl phenol monomer solution, mixing, and magnetically stirring for 20 minutes at room temperature;
fifthly, adding a dimethylol dihydroxy ethylene urea catalyst, adjusting the pH value of the solution to 7.5 by using hydrochloric acid with the concentration of 20 percent, magnetically stirring for 15 minutes until the solution is uniform, and discharging.
The method for processing the artificial forest poplar water-borne functional modifier comprises the following steps:
firstly, diluting the prepared modifier with water until the mass fraction of the modifier solution is 20 percent for later use;
secondly, putting the artificial forest poplar with the water content of less than 10 percent in the specification size of 1000mm multiplied by 200mm multiplied by 25mm into a closed dipping treatment tank, vacuumizing to enable the negative pressure in the tank to be-0.09 MPa, and keeping for 40 minutes;
injecting the modifier liquid medicine into the treatment tank by utilizing the negative pressure effect in the impregnation treatment tank, submerging the wood, relieving the vacuum, carrying out progressive pressurization, pressurizing for 0.2MPa each time, keeping for 20 minutes, repeating for 5 times until the air pressure of 1.0MPa is applied, and keeping for 4 hours;
and fourthly, releasing the pressure of the impregnation treatment tank, discharging the residual modifier, taking out the impregnated wood, and drying in a kiln until the moisture content is 12% to obtain the modified wood.
According to GB/T1927 ~1943 Standard methods such as 2009 test method for physical and mechanical properties of wood are adopted to detect physical and mechanical properties of poplar before and after modification treatment, and the results are as follows: the weight gain rate of the treated wood reaches 37 percent, the water content is 8 percent, and the density is 0.389g/cm before treatment3Increased to 0.691g/cm3(ii) a The anti-expansion rate is improved by more than 57 percent; the bending elastic modulus is increased from 7.9GPa to 13.6 GPa; the bending strength is increased from 57.2MPa to 122.7 MPa; the surface hardness increased from 1130N to 3210N.
The formaldehyde emission of the modified cedarwood is tested according to a dryer method in GB 18580-2001 Formaldehyde emission limits in interior decoration materials, artificial boards and products thereof, and the test value is less than 0.40 mg/L.
According to GB/T2406.2-2009 'determination of combustion behavior by oxygen index method for plastics' test oxygen index before and after modification treatment of fir, the result is: the oxygen index increased from 21% to 49% before treatment.
According to GB/T13942.1-2009 durability of Wood, part 1: the natural corrosion resistance laboratory test method determines the corrosion resistance of the poplar before and after treatment, and the result is as follows: the weight loss rates of the material and the modified poplar material subjected to wood decay by wood decay fungi are 59.6% and 8.9% respectively, which shows that the corrosion resistance of the modified poplar is improved.
Claims (1)
1. The method for treating the water-borne functional modifier for the artificial forest wood is characterized in that the water-borne functional modifier comprises the following components, by weight, 100 parts of phenol, 100 ~ 150 parts of formaldehyde, 80 ~ 150 parts of dimethylol dihydroxy ethylene urea, 10 ~ 30 parts of dimethylol dihydroxy ethylene urea catalyst, 30 ~ 50 parts of silica sol, 25 ~ 35 parts of sodium hydroxide solution and 20 ~ 40 parts of hydrochloric acid solution;
the synthesis method of the modifier comprises the following steps:
adding phenol and 37 mass percent of formaldehyde solution into a reaction kettle, heating and stirring, controlling the temperature range to be 40 ~ 45 ℃, and adjusting the pH value of the solution to 9.0 ~ 10.0.0 by using 30 mass percent of sodium hydroxide solution;
secondly, because the reaction of the phenol and the formaldehyde is an exothermic reaction, the temperature of the mixed solution is quickly raised to 75 ~ 85 ℃, the reaction temperature is controlled and kept for 60 ~ 90 minutes;
regulating the pH of the mixed solution to 8.0 ~ 9.0.0 by using a hydrochloric acid solution with the concentration of 20%, cooling to 30 ~ 40 ℃, and continuously reacting for 20 ~ 30 minutes under the condition of stirring to obtain a hydroxymethyl phenol monomer solution;
adding 10-45% of dimethylol dihydroxy ethylene urea and silica sol into the prepared hydroxymethyl phenol monomer solution, mixing, and magnetically stirring for 10 ~ 20 minutes at room temperature;
adding a dimethylol dihydroxy ethylene urea catalyst, adjusting the pH of the mixed solution to 7.5 ~ 8 by using a hydrochloric acid solution with the concentration of 20%, and magnetically stirring for 10 ~ 15 minutes until the solution is uniform to obtain a water-borne functional modifier;
the method for processing the water-borne functional modifier for the artificial forest wood comprises the following steps:
firstly, diluting the prepared modifier with water, and adjusting the concentration to the required concentration for later use;
secondly, putting the artificial forest wood with the water content of 10 percent or less into a closed dipping treatment tank, vacuumizing to ensure that the negative pressure in the tank is-0.08 ~ -0.01MPa, and keeping for 45 ~ 60 minutes;
thirdly, injecting modifier liquid medicine into the treatment tank by utilizing the negative pressure effect in the dipping treatment tank, submerging the wood, relieving the vacuum, and carrying out progressive pressurization, wherein the pressurization is 0.1 ~ 0.2.2 MPa each time, the maintenance is carried out for 10 ~ 20 minutes, the process is repeated for 5 ~ 15 times until the air pressure of 0.8 ~ 1.5.5 MPa is applied, and the maintenance is carried out for 4 ~ 6 hours;
releasing the pressure of the impregnation treatment tank, discharging the residual modifier, taking out the impregnated wood, and drying in a kiln until the water content is 8 ~ 12%;
the wood of the artificial forest is poplar, fir, pine, eucalyptus and rubber wood.
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| CN110787955A (en) * | 2019-09-17 | 2020-02-14 | 陈秉鸿 | Vacuum infusion process for solid wood |
| CN113510811B (en) * | 2021-04-30 | 2022-10-18 | 中南林业科技大学 | Method for reinforcing poplar wood by compounding 2D resin and sodium silicate |
| CN113400428A (en) * | 2021-06-10 | 2021-09-17 | 广东省林业科学研究院 | Method for enhancing corrosion resistance and termite resistance of wood by using nano zinc oxide |
| CN114213573B (en) * | 2021-12-17 | 2023-05-23 | 中国林业科学研究院木材工业研究所 | Acrylic ester microemulsion wood modifier and preparation method and application thereof |
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| CN104858980A (en) * | 2014-12-23 | 2015-08-26 | 王玉燕 | Wood dipping processing multi-function modifier |
| CN106393347A (en) * | 2016-10-31 | 2017-02-15 | 北京林业大学 | Organic-inorganic functional composite wood modifier and preparation method thereof |
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