CN113699829A - High-performance low-cycle impregnating adhesive and preparation method and use method thereof - Google Patents
High-performance low-cycle impregnating adhesive and preparation method and use method thereof Download PDFInfo
- Publication number
- CN113699829A CN113699829A CN202111017458.4A CN202111017458A CN113699829A CN 113699829 A CN113699829 A CN 113699829A CN 202111017458 A CN202111017458 A CN 202111017458A CN 113699829 A CN113699829 A CN 113699829A
- Authority
- CN
- China
- Prior art keywords
- weight
- parts
- impregnating
- preparation
- performance low
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 49
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 17
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 21
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims description 32
- 239000004359 castor oil Substances 0.000 claims description 31
- 235000019438 castor oil Nutrition 0.000 claims description 31
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000006136 alcoholysis reaction Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000002202 Polyethylene glycol Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 21
- 229920001223 polyethylene glycol Polymers 0.000 claims description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 230000001105 regulatory effect Effects 0.000 claims description 15
- 238000005470 impregnation Methods 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- 125000005442 diisocyanate group Chemical group 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 230000002378 acidificating effect Effects 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical group COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 239000012974 tin catalyst Substances 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical group C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 4
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 abstract description 9
- 239000004814 polyurethane Substances 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 229920005989 resin Polymers 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000006011 modification reaction Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 239000012948 isocyanate Substances 0.000 description 6
- 150000002513 isocyanates Chemical class 0.000 description 6
- 238000004026 adhesive bonding Methods 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/18—Paper- or board-based structures for surface covering
- D21H27/22—Structures being applied on the surface by special manufacturing processes, e.g. in presses
- D21H27/26—Structures being applied on the surface by special manufacturing processes, e.g. in presses characterised by the overlay sheet or the top layers of the structures
- D21H27/28—Structures being applied on the surface by special manufacturing processes, e.g. in presses characterised by the overlay sheet or the top layers of the structures treated to obtain specific resistance properties, e.g. against wear or weather
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/46—Block or graft polymers prepared by polycondensation of aldehydes or ketones on to macromolecular compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/02—Material of vegetable origin
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/07—Nitrogen-containing compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/36—Polyalkenyalcohols; Polyalkenylethers; Polyalkenylesters
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/53—Polyethers; Polyesters
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/57—Polyureas; Polyurethanes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
- D21H17/72—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic material
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
- D21H17/74—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic and inorganic material
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of impregnating compound, in particular to a high-performance low-cycle impregnating compound, a preparation method and a use method thereof, wherein the preparation method comprises the following steps: (1) preparing a polyurethane prepolymer; (2) and (4) preparing the impregnating adhesive. In the synthesis process of the impregnating adhesive, the hydroxyl-terminated polyurethane prepolymer can be subjected to graft modification reaction with melamine under the catalysis of acetic acid, and then continuously reacts with formaldehyde and urea to form semi-interpenetrating network resin, so that the mechanical property of the impregnating adhesive is improved through the characteristics of polyurethane, the curing efficiency is improved through a dense network structure, the formaldehyde consumption is relatively reduced, and the impregnating adhesive is more environment-friendly and safe.
Description
Technical Field
The invention relates to the technical field of impregnating compound, in particular to a high-performance low-cycle impregnating compound and a preparation method and a use method thereof.
Background
The impregnated paper is prepared by taking specially produced base paper as a main material, impregnating the base paper with synthetic resin and drying the impregnated base paper, covering the base paper on the artificial board, and performing hot-pressing adhesion to form decorative paper, so that the aesthetic property of the artificial board is improved. At present, the commonly used synthetic resins of the impregnating compound are mainly phenolic resin, urea resin and melamine formaldehyde resin, wherein the melamine formaldehyde resin becomes the most common impregnating resin with the most extensive application in the market at present due to the higher cost performance of the melamine formaldehyde resin.
However, the melamine formaldehyde resin is brittle, has weak impact resistance, and has a long drying and curing period, so that the application of the melamine formaldehyde resin is greatly limited.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a high-performance low-cycle impregnating adhesive and a preparation method and a using method thereof.
The purpose of the invention is realized by the following technical scheme:
a preparation method of high-performance low-period impregnating adhesive comprises the following steps:
(1) preparing a polyurethane prepolymer: adding 20-30 parts by weight of alcoholysis castor oil, 25-45 parts by weight of polyethylene glycol, 10-30 parts by weight of diisocyanate and 0.1-0.3 part by weight of catalyst into 100 parts by weight of water, heating to 60-70 ℃, and carrying out heat preservation reaction for 3-4h to obtain a hydroxyl-terminated polyurethane prepolymer;
(2) preparing the impregnating adhesive: adding 4-8 parts by weight of acetic acid and 15-25 parts by weight of melamine into 100 parts by weight of polyurethane prepolymer, heating to 80-90 ℃, carrying out heat preservation reaction for 1-2h, cooling to 60-70 ℃, adding 70-80 parts by weight of 35-40% formaldehyde aqueous solution and 20-30 parts by weight of urea, adding an alkaline regulator, regulating the pH value to 8.5-9.5, heating to 80-90 ℃, carrying out heat preservation reaction for 30-60min, then adding an acidic regulator, regulating the pH value to 5.5-6.0, adding 10-20 parts by weight of polyvinyl alcohol, carrying out heat preservation reaction for 20-30min, adding an alkaline regulator, regulating the pH value to 8.0-9.0, then adding 5-15 parts by weight of melamine, continuing heat preservation reaction for 50-60min, cooling to 40-50 ℃, adding 4-6 parts by weight of urea, reacting for 10-20min under heat preservation, and cooling to normal temperature to obtain the dipping glue.
The polyurethane has a discontinuous micro-phase structure formed by the polyol serving as a hard segment and the isocyanate serving as a soft segment, so that the polyurethane can have better hardness and toughness, and the introduction of the polyurethane into the melamine-formaldehyde resin can effectively improve the toughness performance of the impregnated layer. The alcoholysis castor oil has rich sources and low cost, the hydroxyl-terminated polyurethane prepolymer is synthesized by alcoholysis castor oil, polyethylene glycol and isocyanate, the cost of the impregnating adhesive can be effectively controlled, the length of a chain segment of a molecule can be improved by adding the polyethylene glycol, so that the toughness of the impregnating adhesive is more effectively improved, the alcoholysis castor oil and the polyethylene glycol are excessive relative to the isocyanate, the aim of terminating the hydroxyl group is fulfilled, in the synthetic process of the impregnating adhesive, the alcoholysis castor oil and the polyethylene glycol can be subjected to graft modification reaction with melamine under the catalysis of acetic acid and then continuously react with formaldehyde and urea to form semi-interpenetrating network resin, the mechanical property of the impregnating adhesive is improved by virtue of the characteristics of polyurethane, the curing efficiency is improved by virtue of a dense network structure, the consumption of the formaldehyde is relatively reduced, and the impregnating adhesive is more environment-friendly and safe.
The preparation method of the alcoholysis castor oil comprises the following steps: mixing castor oil, glycerol and zinc oxide according to the weight ratio of 100:20-30:0.1-0.3, heating to 240 ℃ and reacting for 1-2h, cooling to 50-60 ℃, and adding xylene for azeotropic dehydration to obtain the alcoholysis castor oil.
Wherein the diisocyanate is diphenylmethane diisocyanate or toluene diisocyanate, and the polyethylene glycol is PEG-400.
Wherein the catalyst is an organic tin catalyst.
Wherein, the polyvinyl alcohol is PVA 17-88.
Wherein the alkaline regulator is a sodium hydroxide solution with the mass fraction of 10-30%, and the acidic regulator is a formic acid solution with the mass fraction of 2-5%.
The high-performance low-cycle impregnating adhesive is prepared by the preparation method of the high-performance low-cycle impregnating adhesive.
A use method of high-performance low-cycle impregnating adhesive comprises the following steps: the base paper is impregnated with the impregnation gum as described above, and after impregnation, the excess impregnation gum is removed by pressing, dried and cooled.
Wherein the gluing amount is 60-80g/m2The drying temperature is 110-120 ℃, and the drying is carried out until the water content of the base paper does not exceed 7 percent.
The invention has the beneficial effects that: the polyurethane has a discontinuous micro-phase structure formed by the polyol serving as a hard segment and the isocyanate serving as a soft segment, so that the polyurethane can have better hardness and toughness, and the introduction of the polyurethane into the melamine-formaldehyde resin can effectively improve the toughness performance of the impregnated layer. The alcoholysis castor oil has rich sources and low cost, the hydroxyl-terminated polyurethane prepolymer is synthesized by alcoholysis castor oil, polyethylene glycol and isocyanate, the cost of the impregnating adhesive can be effectively controlled, the length of a chain segment of a molecule can be improved by adding the polyethylene glycol, so that the toughness of the impregnating adhesive is more effectively improved, the alcoholysis castor oil and the polyethylene glycol are excessive relative to the isocyanate, the aim of terminating the hydroxyl group is fulfilled, in the synthetic process of the impregnating adhesive, the alcoholysis castor oil and the polyethylene glycol can be subjected to graft modification reaction with melamine under the catalysis of acetic acid and then continuously react with formaldehyde and urea to form semi-interpenetrating network resin, the mechanical property of the impregnating adhesive is improved by virtue of the characteristics of polyurethane, the curing efficiency is improved by virtue of a dense network structure, the consumption of the formaldehyde is relatively reduced, and the impregnating adhesive is more environment-friendly and safe.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
A preparation method of high-performance low-period impregnating adhesive comprises the following steps:
(1) preparing a polyurethane prepolymer: adding 25 parts by weight of alcoholysis castor oil, 35 parts by weight of polyethylene glycol, 20 parts by weight of diisocyanate and 0.2 part by weight of catalyst into 100 parts by weight of water, heating to 65 ℃, and carrying out heat preservation reaction for 3.5 hours to obtain a hydroxyl-terminated polyurethane prepolymer;
(2) preparing the impregnating adhesive: adding 6 parts by weight of acetic acid and 20 parts by weight of melamine into 100 parts by weight of polyurethane prepolymer, heating to 85 ℃, carrying out heat preservation reaction for 1.5h, cooling to 65 ℃, adding 75 parts by weight of 35% formaldehyde aqueous solution and 25 parts by weight of urea, adding an alkaline regulator, regulating the pH value to 9.0, heating to 85 ℃, carrying out heat preservation reaction for 45min, then adding an acidic regulator, regulating the pH value to 5.8, adding 15 parts by weight of polyvinyl alcohol, carrying out heat preservation reaction for 25min, adding an alkaline regulator, regulating the pH value to 8.5, then adding 10 parts by weight of melamine, continuing to carry out heat preservation reaction for 55min, cooling to 45 ℃, adding 5 parts by weight of urea, carrying out heat preservation reaction for 15min, and cooling to normal temperature to obtain the impregnating compound.
The preparation method of the alcoholysis castor oil comprises the following steps: mixing castor oil, glycerol and zinc oxide according to the weight ratio of 100:25:0.2, heating to 220 ℃, reacting for 1.5h, cooling to 55 ℃, and adding xylene for azeotropic dehydration to obtain the alcoholysis castor oil.
Wherein the diisocyanate is diphenylmethane diisocyanate, and the polyethylene glycol is PEG-400.
Wherein the catalyst is an organic tin catalyst.
Wherein, the polyvinyl alcohol is PVA 17-88.
The alkaline regulator is a sodium hydroxide solution with the mass fraction of 20%, and the acidic regulator is a formic acid solution with the mass fraction of 3.5%.
The high-performance low-cycle impregnating adhesive is prepared by the preparation method of the high-performance low-cycle impregnating adhesive.
A use method of high-performance low-cycle impregnating adhesive comprises the following steps: the base paper is impregnated with the impregnation gum as described above, and after impregnation, the excess impregnation gum is removed by pressing, dried and cooled.
Wherein the gluing amount is 70g/m2The drying temperature is 110-120 ℃, and the drying is carried out until the water content of the base paper does not exceed 7 percent.
Example 2
A preparation method of high-performance low-period impregnating adhesive comprises the following steps:
(1) preparing a polyurethane prepolymer: adding 20 parts by weight of alcoholysis castor oil, 25 parts by weight of polyethylene glycol, 10 parts by weight of diisocyanate and 0.1 part by weight of catalyst into 100 parts by weight of water, heating to 60 ℃, and carrying out heat preservation reaction for 3 hours to obtain a hydroxyl-terminated polyurethane prepolymer;
(2) preparing the impregnating adhesive: adding 4 parts by weight of acetic acid and 15 parts by weight of melamine into 100 parts by weight of polyurethane prepolymer, heating to 80 ℃, carrying out heat preservation reaction for 1h, cooling to 60 ℃, adding 70 parts by weight of 40% formaldehyde aqueous solution and 20 parts by weight of urea, adding an alkaline regulator, regulating the pH value to 8.5, heating to 80 ℃, carrying out heat preservation reaction for 30min, then adding an acidic regulator, regulating the pH value to 5.5, adding 10 parts by weight of polyvinyl alcohol, carrying out heat preservation reaction for 20min, adding an alkaline regulator, regulating the pH value to 8.0, then adding 5 parts by weight of melamine, continuing the heat preservation reaction for 50min, cooling to 40 ℃, adding 4 parts by weight of urea, carrying out heat preservation reaction for 10min, and cooling to normal temperature to obtain the impregnating compound.
The preparation method of the alcoholysis castor oil comprises the following steps: mixing castor oil, glycerol and zinc oxide according to the weight ratio of 100:20:0.1, heating to 200 ℃, reacting for 1h, cooling to 50 ℃, and adding xylene for azeotropic dehydration to obtain the alcoholysis castor oil.
Wherein the diisocyanate is toluene diisocyanate, and the polyethylene glycol is PEG-400.
Wherein the catalyst is an organic tin catalyst.
Wherein, the polyvinyl alcohol is PVA 17-88.
The alkaline regulator is a sodium hydroxide solution with the mass fraction of 10%, and the acidic regulator is a formic acid solution with the mass fraction of 2%.
The high-performance low-cycle impregnating adhesive is prepared by the preparation method of the high-performance low-cycle impregnating adhesive.
A use method of high-performance low-cycle impregnating adhesive comprises the following steps: the base paper is impregnated with the impregnation gum as described above, and after impregnation, the excess impregnation gum is removed by pressing, dried and cooled.
Wherein the gluing amount is 60g/m2The drying temperature is 110 ℃, and the drying is carried out until the water content of the base paper is not more than 7%.
Example 3
A preparation method of high-performance low-period impregnating adhesive comprises the following steps:
(1) preparing a polyurethane prepolymer: adding 30 parts by weight of alcoholysis castor oil, 45 parts by weight of polyethylene glycol, 30 parts by weight of diisocyanate and 0.3 part by weight of catalyst into 100 parts by weight of water, heating to 70 ℃, and carrying out heat preservation reaction for 4 hours to obtain a hydroxyl-terminated polyurethane prepolymer;
(2) preparing the impregnating adhesive: adding 8 parts by weight of acetic acid and 25 parts by weight of melamine into 100 parts by weight of polyurethane prepolymer, heating to 90 ℃, carrying out heat preservation reaction for 2 hours, cooling to 70 ℃, adding 80 parts by weight of 40% formaldehyde aqueous solution and 30 parts by weight of urea, adding an alkaline regulator, regulating the pH value to 9.5, heating to 90 ℃, carrying out heat preservation reaction for 60 minutes, then adding an acidic regulator, regulating the pH value to 6.0, adding 20 parts by weight of polyvinyl alcohol, carrying out heat preservation reaction for 30 minutes, adding an alkaline regulator, regulating the pH value to 9.0, then adding 15 parts by weight of melamine, continuing the heat preservation reaction for 60 minutes, cooling to 50 ℃, adding 6 parts by weight of urea, carrying out heat preservation reaction for 20 minutes, and cooling to normal temperature to obtain the impregnating compound.
The preparation method of the alcoholysis castor oil comprises the following steps: mixing castor oil, glycerol and zinc oxide according to the weight ratio of 100:30:0.3, heating to 240 ℃, reacting for 2h, cooling to 60 ℃, and adding xylene for azeotropic dehydration to obtain the alcoholysis castor oil.
Wherein the diisocyanate is diphenylmethane diisocyanate, and the polyethylene glycol is PEG-400.
Wherein the catalyst is an organic tin catalyst.
Wherein, the polyvinyl alcohol is PVA 17-88.
The alkaline regulator is a sodium hydroxide solution with the mass fraction of 30%, and the acidic regulator is a formic acid solution with the mass fraction of 5%.
The high-performance low-cycle impregnating adhesive is prepared by the preparation method of the high-performance low-cycle impregnating adhesive.
A use method of high-performance low-cycle impregnating adhesive comprises the following steps: the base paper is impregnated with the impregnation gum as described above, and after impregnation, the excess impregnation gum is removed by pressing, dried and cooled.
Wherein the gluing amount is 80g/m2Drying at 120 deg.C until the water content of the base paper is not more than 7%.
Comparative example 1
This comparative example differs from example 1 in that:
preparing a polyurethane prepolymer: adding 60 parts by weight of polyethylene glycol, 30 parts by weight of diisocyanate and 0.3 part by weight of catalyst into 100 parts by weight of water, heating to 70 ℃, and carrying out heat preservation reaction for 4 hours to obtain hydroxyl-terminated polyurethane prepolymer
Comparative example 2
This comparative example differs from example 1 in that:
preparing a polyurethane prepolymer: adding 50 parts by weight of alcoholysis castor oil, 30 parts by weight of diisocyanate and 0.3 part by weight of catalyst into 100 parts by weight of water, heating to 70 ℃, and carrying out heat preservation reaction for 4 hours to obtain the hydroxyl-terminated polyurethane prepolymer.
The impregnated papers of example 1 and comparative examples 1-3 were subjected to formation testing, with the following test indices and methods:
tensile strength: GB/T13022-1991
Impact strength: GB/T1843-2008
Surface bonding strength: GB/T15102-2006
Formaldehyde emission: GB/T17657-2013 climate box method
| Example 1 | Comparative example 1 | Comparative example 2 | |
| Tensile Strength (MPa) | 68.5 | 58.3 | 62.2 |
| Impact strength (KJ/m)2) | 3.36 | 2.09 | 1.88 |
| Surface bonding Strength (MPa) | 2.68 | 2.45 | 2.31 |
| Formaldehyde emission (mg/L) | 1.07 | 1.09 | 1.04 |
As can be seen from comparison among examples 1, comparative examples 1 and 2, the melamine-formaldehyde resin can be modified by the hydroxyl-terminated polyurethane prepolymer, but the tensile strength and impact strength of the polyurethane prepolymer only using polyethylene glycol or alcoholysis castor oil as a hard segment are not significantly improved, and particularly the impact strength of the comparative example 2 is reduced more obviously, which shows that the polyhydroxy characteristic of alcoholysis castor oil improves the branching degree of a network structure, so that the hardness of the impregnating adhesive is improved, but the toughness is reduced, and the length of a linear molecular chain segment can be extended by the matching of polyethylene glycol, so that the strength and the toughness are better improved.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (9)
1. A preparation method of high-performance low-period impregnating adhesive is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a polyurethane prepolymer: adding 20-30 parts by weight of alcoholysis castor oil, 25-45 parts by weight of polyethylene glycol, 10-30 parts by weight of diisocyanate and 0.1-0.3 part by weight of catalyst into 100 parts by weight of water, heating to 60-70 ℃, and carrying out heat preservation reaction for 3-4h to obtain a hydroxyl-terminated polyurethane prepolymer;
(2) preparing the impregnating adhesive: adding 4-8 parts by weight of acetic acid and 15-25 parts by weight of melamine into 100 parts by weight of polyurethane prepolymer, heating to 80-90 ℃, carrying out heat preservation reaction for 1-2h, cooling to 60-70 ℃, adding 70-80 parts by weight of 35-40% formaldehyde aqueous solution and 20-30 parts by weight of urea, adding an alkaline regulator, regulating the pH value to 8.5-9.5, heating to 80-90 ℃, carrying out heat preservation reaction for 30-60min, then adding an acidic regulator, regulating the pH value to 5.5-6.0, adding 10-20 parts by weight of polyvinyl alcohol, carrying out heat preservation reaction for 20-30min, adding an alkaline regulator, regulating the pH value to 8.0-9.0, then adding 5-15 parts by weight of melamine, continuing heat preservation reaction for 50-60min, cooling to 40-50 ℃, adding 4-6 parts by weight of urea, reacting for 10-20min under heat preservation, and cooling to normal temperature to obtain the dipping glue.
2. The preparation method of the high-performance low-cycle impregnating adhesive according to claim 1, which is characterized in that: the preparation method of the alcoholysis castor oil comprises the following steps: mixing castor oil, glycerol and zinc oxide according to the weight ratio of 100:20-30:0.1-0.3, heating to 240 ℃ and reacting for 1-2h, cooling to 50-60 ℃, and adding xylene for azeotropic dehydration to obtain the alcoholysis castor oil.
3. The preparation method of the high-performance low-cycle impregnating adhesive according to claim 1, which is characterized in that: the diisocyanate is diphenylmethane diisocyanate or toluene diisocyanate, and the polyethylene glycol is PEG-400.
4. The preparation method of the high-performance low-cycle impregnating adhesive according to claim 1, which is characterized in that: the catalyst is an organic tin catalyst.
5. The preparation method of the high-performance low-cycle impregnating adhesive according to claim 1, which is characterized in that: the polyvinyl alcohol is PVA 17-88.
6. The preparation method of the high-performance low-cycle impregnating adhesive according to claim 1, which is characterized in that: the alkaline regulator is a sodium hydroxide solution with the mass fraction of 10-30%, and the acidic regulator is a formic acid solution with the mass fraction of 2-5%.
7. A high-performance low-period impregnating adhesive is characterized in that: the preparation method of the high-performance low-cycle impregnating adhesive is characterized by comprising the following steps of 1-6.
8. A use method of high-performance low-period impregnating adhesive is characterized by comprising the following steps: impregnating the base paper with the impregnating glue of claim 7, pressing to remove excess impregnating glue after impregnation, drying and cooling.
9. The use method of the high-performance low-cycle impregnating adhesive according to claim 8, characterized in that: the glue applying amount is 60-80g/m2The drying temperature is 110-120 ℃, and the drying is carried out until the water content of the base paper does not exceed 7 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111017458.4A CN113699829A (en) | 2021-08-31 | 2021-08-31 | High-performance low-cycle impregnating adhesive and preparation method and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111017458.4A CN113699829A (en) | 2021-08-31 | 2021-08-31 | High-performance low-cycle impregnating adhesive and preparation method and use method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113699829A true CN113699829A (en) | 2021-11-26 |
Family
ID=78658443
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111017458.4A Pending CN113699829A (en) | 2021-08-31 | 2021-08-31 | High-performance low-cycle impregnating adhesive and preparation method and use method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113699829A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508938A (en) * | 2009-02-25 | 2009-08-19 | 南京红宝丽股份有限公司 | Structure type flame-proof polyol prepared with ricinus oil and uses in polyurethane foam plastics |
| CN103160231A (en) * | 2013-03-26 | 2013-06-19 | 成都帝龙新材料有限公司 | Adhesive and application method thereof for sticky membrane paper |
| CN104893633A (en) * | 2015-05-25 | 2015-09-09 | 西南林业大学 | Melamine-urea-formaldehyde copolycondensation resin adhesive for laminated wood and preparation method thereof |
| CN108276942A (en) * | 2018-01-24 | 2018-07-13 | 南宁科天水性科技有限责任公司 | A kind of ultralow aldehyde impregnated paper dipping glue and preparation method thereof |
| CN109355968A (en) * | 2018-10-11 | 2019-02-19 | 广东福美新材料科技有限公司 | A kind of wearable environment protection type impregnated paper and preparation method thereof |
| CN109354824A (en) * | 2018-09-29 | 2019-02-19 | 湖南邦弗特新材料技术有限公司 | A kind of aqueous photo-curing modified melamine-formaldehyde impregnating resin and preparation method thereof |
| CN109851720A (en) * | 2019-02-15 | 2019-06-07 | 临沂市鲁源浸渍纸业有限公司 | A kind of no aldehyde dipping glue and its synthesis technology |
| CN110408001A (en) * | 2019-06-21 | 2019-11-05 | 黄兰英 | A kind of preparation method of water-based polyurethane curing agent |
| CN111300568A (en) * | 2019-12-16 | 2020-06-19 | 唐文夺 | Modified melamine formaldehyde resin impregnation liquid and preparation method and application thereof |
| CN111531660A (en) * | 2020-05-09 | 2020-08-14 | 中国林业科学研究院木材工业研究所 | Low-formaldehyde impregnated bond paper facing artificial board and preparation method thereof |
-
2021
- 2021-08-31 CN CN202111017458.4A patent/CN113699829A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508938A (en) * | 2009-02-25 | 2009-08-19 | 南京红宝丽股份有限公司 | Structure type flame-proof polyol prepared with ricinus oil and uses in polyurethane foam plastics |
| CN103160231A (en) * | 2013-03-26 | 2013-06-19 | 成都帝龙新材料有限公司 | Adhesive and application method thereof for sticky membrane paper |
| CN104893633A (en) * | 2015-05-25 | 2015-09-09 | 西南林业大学 | Melamine-urea-formaldehyde copolycondensation resin adhesive for laminated wood and preparation method thereof |
| CN108276942A (en) * | 2018-01-24 | 2018-07-13 | 南宁科天水性科技有限责任公司 | A kind of ultralow aldehyde impregnated paper dipping glue and preparation method thereof |
| CN109354824A (en) * | 2018-09-29 | 2019-02-19 | 湖南邦弗特新材料技术有限公司 | A kind of aqueous photo-curing modified melamine-formaldehyde impregnating resin and preparation method thereof |
| CN109355968A (en) * | 2018-10-11 | 2019-02-19 | 广东福美新材料科技有限公司 | A kind of wearable environment protection type impregnated paper and preparation method thereof |
| CN109851720A (en) * | 2019-02-15 | 2019-06-07 | 临沂市鲁源浸渍纸业有限公司 | A kind of no aldehyde dipping glue and its synthesis technology |
| CN110408001A (en) * | 2019-06-21 | 2019-11-05 | 黄兰英 | A kind of preparation method of water-based polyurethane curing agent |
| CN111300568A (en) * | 2019-12-16 | 2020-06-19 | 唐文夺 | Modified melamine formaldehyde resin impregnation liquid and preparation method and application thereof |
| CN111531660A (en) * | 2020-05-09 | 2020-08-14 | 中国林业科学研究院木材工业研究所 | Low-formaldehyde impregnated bond paper facing artificial board and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111531658B (en) | Preparation method of impregnated bond paper facing formaldehyde-free artificial board | |
| CN102086257A (en) | Environment-friendly urea resin for laminating plywoods from high water-content veneers and preparation and application thereof | |
| CN111531660B (en) | Low-formaldehyde impregnated bond paper facing artificial board and preparation method thereof | |
| CN111501416B (en) | Formaldehyde-free impregnation adhesive for decorative paper and preparation method thereof | |
| CN114134751B (en) | Waterproof composite resin for surface impregnation of reinforced wood floor and preparation method thereof | |
| CN100500723C (en) | Environment friendly quaternarily copolymerized thermosetting copolymer resin for high pressure laminated decorative board | |
| CA3234147A1 (en) | Preparation method for veneer manufactured board | |
| CN113699829A (en) | High-performance low-cycle impregnating adhesive and preparation method and use method thereof | |
| CN111635722B (en) | Low-temperature curing ultralow-aldehyde water-resistant composite adhesive and preparation method thereof | |
| CN112606127A (en) | Compound environmental protection ecological plate of multilayer | |
| CN110615880B (en) | Epoxy compound and polyol prepolymer modified urea-formaldehyde resin and preparation method thereof | |
| CN114670294B (en) | High-strength ecological plate and manufacturing process | |
| CN113308213B (en) | Anticorrosive and flame-retardant aldehyde-free plywood and preparation method thereof | |
| CN116065419A (en) | Preparation technology for improving brittleness of melamine impregnated paper | |
| CN113389082B (en) | Long-acting low-formaldehyde impregnated paper and preparation method thereof | |
| CN114015001A (en) | Preparation method of phenolic resin | |
| HU215944B (en) | Method of producing highly reactive uera-modified phenolic resins for use as core-chip binders in the manufacture of chipboards | |
| CN113861851A (en) | Biomass aldehyde-free glue and preparation method thereof | |
| CN111073579B (en) | High-initial-viscosity polyurethane adhesive for artificial board and preparation method and application thereof | |
| CN113463432A (en) | Antibacterial odor-removing impregnated paper and preparation method thereof | |
| CN103666350A (en) | Maltose-melamine-formaldehyde copolycondensation resin wood adhesive and preparation method thereof | |
| CN112300350B (en) | Urea-formaldehyde resin adhesive modifier and application thereof, modified urea-formaldehyde resin adhesive and application thereof | |
| CN115353850B (en) | Environment-friendly waterproof tannin-based wood adhesive and preparation method thereof | |
| CN116478647B (en) | Preparation method of mixed resin for steam-induced-cured ENF-grade shaving board | |
| CN114030039B (en) | High-strength ecological board without added aldehyde and production process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220622 Address after: 523000 No. 45, Jinshan Road, Chashan Town, Dongguan City, Guangdong Province Applicant after: GUANGDONG FUMEI NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: 526200 room 219-3, second floor, No. 9, Huiyuan Avenue, longfu Town, Sihui City, Zhaoqing City, Guangdong Province Applicant before: Guangdong Zhaoqing Fumei Decoration Material Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211126 |
|
| RJ01 | Rejection of invention patent application after publication |