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CN-119658790-B - Preparation process of high-performance green flame-retardant plywood

CN119658790BCN 119658790 BCN119658790 BCN 119658790BCN-119658790-B

Abstract

The invention relates to a preparation process of a high-performance green flame-retardant plywood, which comprises the following steps: the preparation method creatively combines preparation methods such as esterification reaction, reverse conversion method, chemical one-step method, hot pressing method and the like, and the prepared high-performance green flame-retardant plywood has the advantages of good mechanical property, excellent flame retardance and the like, and has the characteristics of wide raw material sources, strong reproducibility, high reactivity and the like, is compounded with a green environment-friendly concept, and has wide application prospect in plywood application fields.

Inventors

  • LU YUBAO

Assignees

  • 广西剑鑫木业集团有限公司

Dates

Publication Date
20260508
Application Date
20241209

Claims (7)

  1. 1. The preparation technology of the high-performance green flame-retardant plywood is characterized by comprising the steps of synthesis of a cross-linking agent furan dicarboxylic acid-NHS active ester (FDCA-NHS), preparation of a high Wen Pojiao adhesive, preparation of water-based epoxy resin, preparation of an L-Trp-DOPO inorganic phosphorus-containing flame retardant, preparation of an epoxy resin flame-retardant material and preparation of the high-performance green flame-retardant plywood, wherein: step (1) Synthesis of crosslinker furandicarboxylic acid-NHS active ester (FDCA-NHS) Dissolving 2, 5-furan dicarboxylic acid (FDCA) and N-hydroxysuccinimide (NHS) in dimethyl sulfoxide (DMSO), adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide (EDC), stirring at a certain temperature, washing dimethyl sulfoxide (DMSO) by an extraction method after the reaction is finished, purifying a reaction product by column chromatography, and finally drying in a vacuum drying oven at a certain temperature for later use; preparation of Gao Wenpo adhesive in step (2) Taking flaky soybean meal, putting the soybean meal into a pulverizer to pulverize, sieving the soybean meal to obtain soybean meal powder, adding water into the solution of the cross-linking agent furan dicarboxylic acid-NHS active ester (FDCA-NHS) obtained in the step (1), stirring the mixture uniformly at room temperature, adjusting the solid content of a solvent, adding the soybean meal powder, and stirring the mixture at room temperature to form a uniform soybean meal adhesive without particles, thereby obtaining a high Wen Pojiao adhesive; Preparation of the waterborne epoxy resin in the step (3) Adding epoxy resin E-31 and polyethylene glycol (PEG) into a three-neck flask with a stirrer and a condenser tube, heating to raise the temperature, stirring and mixing uniformly after the mixture is melted, slowly dripping potassium persulfate into the flask after the potassium persulfate is dissolved in water, mixing uniformly, raising the temperature to obtain a nonionic epoxy emulsifier, lowering the temperature, adding epoxy resin E-54, stirring to uniformly mix the epoxy emulsifier with the epoxy emulsifier, slowly dripping distilled water at a certain stirring speed, changing the system from W/O to O/W when the viscosity of the system suddenly drops, and continuing stirring for a period of time after the water is added to obtain the water-based epoxy resin; step (4) preparation of L-Trp-DOPO inorganic phosphorus-containing flame retardant Weighing a certain amount of L-Trp-BS and an organic phosphorus compound (DOPO), dissolving in a three-necked flask filled with tetrahydrofuran, fully stirring, putting the mixed solution into an oil bath pot, reacting for a period of time, washing the precipitated dark yellow product by ethanol and deionized water, and drying overnight in a blast oven at a certain temperature to obtain the L-Trp-DOPO inorganic phosphorus-containing flame retardant; preparation of epoxy resin flame-retardant material in step (5) Dissolving the flame retardant L-Trp-DOPO prepared in the step (4) in absolute ethyl alcohol, fully dispersing in water bath for a period of time, adding the epoxy resin obtained in the step (3) to stir, adding diethylenetriamine into the mixed solution, pumping the absolute ethyl alcohol out of a vacuum filter, pouring the mixed solution into a preheating template after a period of time, removing bubbles in a baking oven, placing a sample in the baking oven for curing for a period of time, and transferring the baking oven into a temperature programming storage; preparation of high-performance green flame-retardant plywood in step (6) The method comprises the steps of using five layers of eucalyptus veneers, using the high Wen Pojiao adhesive obtained in the step (2), adding the epoxy resin flame retardant material obtained in the step (5), setting a proper single-sided adhesive coating amount, using a pre-pressing process, setting unit pressure, cold pressing for a period of time, setting hot pressing temperature and unit pressure, hot pressing for a period of time, exhausting the unit pressure (0.2+/-0.1) MPa, and obtaining the high-performance green flame-retardant plywood after the exhausting time is finished.
  2. 2. The process for preparing the high-performance green flame-retardant plywood is characterized in that: step (1) Synthesis of crosslinker furandicarboxylic acid-NHS active ester (FDCA-NHS) 2.8-3.1 Mmol of 2, 5-furandicarboxylic acid (FDCA) and 5.6-7.1 mmol of N-hydroxysuccinimide (NHS) are dissolved in 15-23 mL of dimethyl sulfoxide (DMSO), 5.6-6.9 mmol of 1-ethyl- (3-dimethylaminopropyl) carbodiimide (EDC) is added into the solution, the mixed reaction solution is stirred for 48-56 h at 25-35 ℃, after the reaction is finished, the dimethyl sulfoxide (DMSO) is washed off by an extraction method, the reaction product is purified by a column chromatography method, and finally the reaction product is dried in a vacuum drying box at 50-60 ℃ for standby.
  3. 3. The process for preparing the high-performance green flame-retardant plywood is characterized in that: preparation of Gao Wenpo adhesive in step (2) And (3) putting the flaky soybean meal into a pulverizer to pulverize for 5-8 min, sieving the soybean meal with a 160-200 mesh screen to obtain soybean meal powder, taking 89.55-91.65 g of the cross-linking agent furandicarboxylic acid-NHS active ester (FDCA-NHS) solution (13.4-15.6wt%) obtained in the step (1), adding 10.45-11.95 g of water into the solution, stirring the mixture uniformly at room temperature to adjust the solid content of the solvent to 12.0-13.0wt%, adding 30.00-35.00 g of soybean meal powder, and stirring the mixture for 3-5 min at room temperature to form the soybean meal adhesive with the solid content of 30-35 wt% and even no particles, thereby obtaining the high Wen Pojiao adhesive.
  4. 4. A process for preparing a high-performance green flame-retardant plywood according to claim 3, which is characterized in that: Preparation of the waterborne epoxy resin in the step (3) Adding epoxy resin E-31 and polyethylene glycol (PEG) into a 250-300 mL three-neck flask with a stirrer and a condenser tube, heating to 80-90 ℃, stirring and mixing uniformly after the epoxy resin E-31 and the polyethylene glycol (PEG) are melted, slowly dripping potassium persulfate into the flask after the potassium persulfate is dissolved in water, mixing uniformly for 30-35 min, heating to obtain a nonionic epoxy emulsifier, reducing the temperature to 70-75 ℃, adding epoxy resin E-54, stirring for 30-35 min to uniformly mix the epoxy emulsifier and the epoxy emulsifier, slowly dripping distilled water at a stirring speed of 1000-1200 r/min, changing the system from W/O to O/W when the viscosity of the system suddenly drops, and continuing stirring for 30-35 min after the water is added to obtain the aqueous epoxy resin with the solid content of 50-52%.
  5. 5. The process for preparing the high-performance green flame-retardant plywood is characterized in that: step (4) preparation of L-Trp-DOPO inorganic phosphorus-containing flame retardant 1.42-1.86 G of L-Trp-BS and 0.75-1 g of organic phosphorus compound (DOPO) are weighed and dissolved in a three-neck flask filled with 45-55 mL of tetrahydrofuran, the three-neck flask is fully stirred, the mixed solution is placed in an oil bath pot at 110-120 ℃ for reaction for 12-14 hours, the precipitated dark yellow product is washed by ethanol and deionized water, and the mixture is dried in a blast oven at 60-65 ℃ overnight, so that the L-Trp-DOPO inorganic phosphorus-containing flame retardant is obtained.
  6. 6. The process for preparing the high-performance green flame-retardant plywood is characterized in that: preparation of epoxy resin flame-retardant material in step (5) Dissolving the flame retardant L-Trp-DOPO prepared in the step (4) in 15-20 mL of absolute ethyl alcohol, fully dispersing in 70-75 ℃ water bath for 15-20 min, adding 30-35 mL of the epoxy resin obtained in the step (3), stirring for 30-45 min, adding 3.4-4.2 mL of diethylenetriamine into the mixed solution, pumping the absolute ethyl alcohol out by a vacuum filter for 5-7 min, pouring the mixed solution into a preheating template, removing bubbles in an 80-90 ℃ oven, placing a sample in the 80-90 ℃ oven for curing for 30-35 min, and then transferring the oven to a temperature programming step to 110-115 ℃ for 3-4 h.
  7. 7. The process for preparing the high-performance green flame-retardant plywood is characterized in that: preparation of high-performance green flame-retardant plywood in step (6) The method comprises the steps of using five layers of eucalyptus veneers, using a high Wen Pojiao adhesive obtained in the step (2), adding the epoxy resin flame retardant material obtained in the step (5) at the same time, and enabling single-sided adhesive coating quantity (260+/-10) g/m 2 , using a pre-pressing process, wherein the pre-pressing process comprises unit pressure (0.7+/-0.1) MPa, cold pressing time l-1.5 h, hot pressing temperature is 125-150 ℃, unit pressure (0.7+/-0.1) MPa, hot pressing time 780-800 s and exhaust time 120-130 s, so that the high-performance green flame-retardant plywood is obtained.

Description

Preparation process of high-performance green flame-retardant plywood Technical Field The invention relates to preparation of a new material, in particular to a preparation process of a high-performance green flame-retardant plywood. Background With the rapid development of the artificial board industry, the environment-friendly performance of the adhesive can be widely focused by consumers, the synthetic resin adhesive taking petrochemical products as raw materials has excellent adhesive performance and water resistance, but some synthetic resins contain substances such as formaldehyde, phenol and the like, which cause harm to the environment and human health in the production, transportation and use processes, the development of the safe and environment-friendly adhesive becomes the research focus and the future development trend of the current adhesive, the environment-friendly and renewable plant protein adhesive is valued and favored by the industries, the wood has combustibility, the artificial board used in the building decoration has fire hazard, the fire-retardant performance of the artificial board becomes one of the main factors selected by consumers along with the implementation of relevant regulations and standard systems of the fire-retardant materials in China. The invention utilizes soybean protein to prepare the green flame-retardant plywood, adopts high-temperature meal to replace low-temperature meal to prepare the soybean meal adhesive, can obviously improve the defects of adhesive bonding strength and water resistance of the adhesive, has the characteristics of (1) strong regeneration capability, and (2) high reaction activity, accords with the green concept, effectively improves the resistance of the soybean meal to normal aging and the storage stability of the soybean meal, simultaneously effectively reduces the raw material cost of the adhesive, combines with the novel composite flame retardant to prepare the green flame-retardant plywood, and has good flame retardance, thereby having positive significance for the development of the application field of the green flame-retardant plywood and the popularization and application of the soybean meal adhesive in the wood industry. Disclosure of Invention Aiming at the problems, the invention provides a preparation process of a high-performance green flame-retardant plywood. The invention provides a preparation process of a high-performance green flame-retardant plywood, which comprises the following steps of synthesis of a cross-linking agent furan dicarboxylic acid-NHS active ester (FDCA-NHS), preparation of a high Wen Pojiao adhesive, preparation of water-based epoxy resin, preparation of an L-Trp-DOPO inorganic phosphorus-containing flame retardant, preparation of an epoxy resin flame-retardant material and preparation of the high-performance green flame-retardant plywood. Wherein, the preparation of the L-Trp-DOPO inorganic phosphorus-containing flame retardant in the step (4) Weighing a certain amount of L-Trp-BS and an organic phosphorus compound (DOPO), dissolving in a three-necked flask filled with tetrahydrofuran, fully stirring, putting the mixed solution into an oil bath pot, reacting for a period of time, washing the precipitated dark yellow product by ethanol and deionized water, and drying overnight in a blast oven at a certain temperature to obtain the L-Trp-DOPO inorganic phosphorus-containing flame retardant; preparation of epoxy resin flame-retardant material in step (5) Dissolving the flame retardant L-Trp-DOPO prepared in the step (4) in absolute ethyl alcohol, fully dispersing in a water bath for a period of time, adding the epoxy resin obtained in the step (3) for stirring, adding diethylenetriamine into the mixed solution, pumping the absolute ethyl alcohol out of a vacuum filter, pouring the mixed solution into a preheating template after a period of time, removing bubbles in a baking oven, placing a sample in the baking oven for curing for a period of time, and transferring the baking oven into a temperature programming storage. Preferably, step (1) Synthesis of the crosslinker furandicarboxylic acid-NHS active ester (FDCA-NHS) Dissolving 2, 5-furan dicarboxylic acid (FDCA) and N-hydroxysuccinimide (NHS) in dimethyl sulfoxide (DMSO), adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide (EDC) into the solution, stirring the mixed reaction solution at a certain temperature, washing the dimethyl sulfoxide (DMSO) by an extraction method after the reaction is finished, purifying the reaction product by a column chromatography method, and finally drying in a vacuum drying oven at a certain temperature for later use; preparation of Gao Wenpo adhesive in step (2) Taking flaky soybean meal, putting the soybean meal into a pulverizer to pulverize, sieving the soybean meal to obtain high-temperature soybean meal powder, adding water into the cross-linking agent modifier furan dicarboxylic acid-NHS active ester (FDCA-NHS) solu