CN112194768A - Water-based phenolic resin and preparation method thereof - Google Patents
Water-based phenolic resin and preparation method thereof Download PDFInfo
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- CN112194768A CN112194768A CN202011044429.2A CN202011044429A CN112194768A CN 112194768 A CN112194768 A CN 112194768A CN 202011044429 A CN202011044429 A CN 202011044429A CN 112194768 A CN112194768 A CN 112194768A
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- formaldehyde
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 37
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 156
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 129
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 69
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 40
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 30
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004202 carbamide Substances 0.000 claims abstract description 28
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 23
- 238000007789 sealing Methods 0.000 claims abstract description 19
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 13
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960002887 deanol Drugs 0.000 claims abstract description 12
- 239000012972 dimethylethanolamine Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 39
- 238000002347 injection Methods 0.000 claims description 27
- 239000007924 injection Substances 0.000 claims description 27
- 239000003513 alkali Substances 0.000 claims description 17
- 239000003638 chemical reducing agent Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 14
- 239000000839 emulsion Substances 0.000 claims description 12
- 238000010793 Steam injection (oil industry) Methods 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 230000007246 mechanism Effects 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 3
- 125000003003 spiro group Chemical group 0.000 claims description 3
- 239000003518 caustics Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 7
- 238000007600 charging Methods 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 5
- 238000005507 spraying Methods 0.000 abstract description 4
- 238000006482 condensation reaction Methods 0.000 abstract description 3
- 238000010583 slow cooling Methods 0.000 abstract description 3
- 238000007259 addition reaction Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 239000012670 alkaline solution Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 7
- 238000005070 sampling Methods 0.000 description 7
- 238000007792 addition Methods 0.000 description 6
- 239000002585 base Substances 0.000 description 4
- CQRYARSYNCAZFO-UHFFFAOYSA-N salicyl alcohol Chemical compound OCC1=CC=CC=C1O CQRYARSYNCAZFO-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 229920001807 Urea-formaldehyde Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- 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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
- C08G14/08—Ureas; Thioureas
-
- 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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a water-based phenolic resin and a preparation method thereof, wherein the water-based phenolic resin comprises the following raw materials in parts by weight: 75-80 parts of formaldehyde solution, 30-32 parts of phenol, 45-50 parts of urea, 0.1 part of caustic soda flakes, 0.1 part of sodium hydroxide solution, 0.4 part of sodium carbonate, 2 parts of triethylamine, 1 part of N-methylethanolamine, 1 part of 2-dimethylethanolamine, 0.01 part of oxalic acid and 50-70 parts of deionized water; the preparation method comprises the following steps: step one, weighing, charging and sealing; step two, preheating and dripping raw materials; step three, heating to carry out addition reaction; cooling to carry out condensation reaction; fifthly, stirring and radiating; the invention solves the problem of kettle spraying caused by too fast temperature rise rate and too late cooling in the prior art, solves the problem of 'kettle forming' caused by longer reaction time and high product molecular weight and viscosity in the prior art, and solves the problems of slow cooling of the reaction kettle and untimely reaction heat conduction in the kettle.
Description
Technical Field
The invention belongs to the technical field of phenolic resin preparation, and particularly relates to a water-based phenolic resin and a preparation method thereof.
Background
The liquid phenolic resin is a yellow, dark brown liquid, such as: the alkaline phenolic resin is mainly used as a casting adhesive. Water-soluble phenol resins or alcohol-soluble phenol resins are used to impregnate paper, cotton, glass, asbestos and other similar materials to provide them with mechanical strength, electrical properties, etc. Typical examples include electrical insulation and mechanical lamination manufacturing, clutch plates and filter paper for automotive filters.
The production of the water-based phenolic resin is carried out by reacting phenol and formaldehyde under the action of an alkaline catalyst, the reaction is exothermic, steam is needed to heat at the initial stage of the reaction, if the temperature is increased too fast, the reaction speed is accelerated rapidly, the cooling is not in time, the boiling is easy to cause, and the kettle spraying phenomenon occurs; in the condensation reaction process, if the stirring is stopped midway or the cooling water is supplied badly, the reaction heat can not be removed in time, the temperature in the kettle can be increased greatly, the material is flushed, and the accident is caused; in addition, the reaction time also directly influences the molecular weight of a product, the longer the reaction time is, the larger the molecular weight is, the higher the viscosity is, and if the reaction time is not controlled, the 'pan-forming' can be caused, so that the heat transfer is influenced, and if the reaction heat cannot be timely led out, the local overheating of a reaction kettle or the overhigh temperature in the kettle can be caused, so that an explosion accident can be caused.
Disclosure of Invention
The invention aims to provide a water-based phenolic resin and a preparation method thereof, which solve the problem of kettle spraying caused by too fast temperature rise rate and too slow cooling in the prior art, solve the problem of 'kettle forming' caused by longer reaction time and high product molecular weight and high viscosity in the prior art, and solve the problems of slow cooling of a reaction kettle and untimely reaction heat conduction in the kettle.
The purpose of the invention can be realized by the following technical scheme:
the water-based phenolic resin comprises the following raw materials in parts by weight: 75-80 parts of formaldehyde solution, 30-32 parts of phenol, 45-50 parts of urea, 0.1 part of caustic soda flakes, 0.1 part of sodium hydroxide solution, 0.4 part of sodium carbonate, 2 parts of triethylamine, 1 part of N-methylethanolamine, 1 part of 2-dimethylethanolamine, 0.01 part of oxalic acid and 50-70 parts of deionized water.
The formaldehyde solution is 44% formaldehyde aqueous solution, and the sodium hydroxide solution is 40-42% sodium hydroxide aqueous solution.
A preparation method of water-based phenolic resin specifically comprises the following steps:
the method comprises the following steps: triethylamine, 2-dimethylethanolamine, N-methylethanolamine, phenol and sodium carbonate are added into a tank body from a feed port of a closed reaction kettle respectively according to the weight part ratio, then a feed cover is closed, and the feed cover and the feed port are locked and closed through a screw and a nut;
step two: injecting clear water between the tank body and the jacket cylinder to a water outlet through a water injection and steam adding port, then injecting steam between the tank body and the jacket cylinder from the water injection and steam adding port, heating the clear water between the tank body and the jacket cylinder by the steam, heating the tank body by the clear water, controlling the temperature in the tank body to be kept at 60-65 ℃, adding a sodium hydroxide solution into the tank body from an alkaline solution dropping port through a closed pipeline, adding a formaldehyde solution into the tank body from the formaldehyde dropping port through the closed pipeline, adjusting valves on the formaldehyde dropping port and the alkaline solution dropping port, and controlling the dropping time of the sodium hydroxide solution and the formaldehyde solution to be 1.5-2 h;
step three: after the dropwise addition of the sodium hydroxide solution and the formaldehyde solution is finished, heating to 75 ℃ at the heating rate of 0.5 ℃/min, then injecting cooling water from a water injection steam inlet, discharging hot water from a water discharge port, keeping the temperature in the tank body at 75 ℃, and preserving the temperature for 4 hours to generate emulsion;
step four: continuously injecting cooling water from a water injection and steam adding port, discharging hot water from a water discharge port, and when the temperature of the emulsion is reduced to 60-65 ℃, respectively injecting the flake caustic soda and the urea into the tank body from a flake caustic soda feed port and a urea feed port through closed pipelines;
step five: adding oxalic acid into the tank body from an oxalic acid charging port through a closed pipeline; adding deionized water into the tank body from the water inlet through a closed pipeline, then starting a motor, stirring at the rotating speed of 600 plus materials at 800r/min, and stopping stirring when the temperature in the tank body is reduced to 25 ℃ to generate the water-based phenolic resin product.
The closed reaction kettle in the steps comprises a tank body, a jacket cylinder, a stirring mechanism and supports, wherein the jacket cylinder is sleeved at the bottom end outside the tank body, the jacket cylinder and the tank body are fixed in a sealing manner, the stirring mechanism penetrates through the top end of the tank body, the supports are uniformly distributed on one side, far away from the tank body, of the jacket cylinder, and the supports are fixed above the side wall of the jacket cylinder;
the device comprises a tank body, a feed inlet, a fixed seat, a through hole, a viewing port, a transparent sealing plate, a slice alkali feed inlet and a water inlet, wherein the feed inlet is arranged on one side of the top end of the tank body, the feed inlet is fixedly communicated with the tank body, the fixed seat is arranged in the center of the top end of the tank body, the through hole penetrates through the top end of the tank body, the viewing port is arranged on one side of the fixed seat, which is away from the feed inlet, the viewing port penetrates through the top end of the tank body and is fixedly connected with the tank body, the transparent sealing plate is arranged in the center of the viewing port, the slice alkali feed inlet and the water inlet are oppositely arranged on two sides of the fixed seat, the slice alkali feed inlet and the bottom end of the water inlet are respectively and fixedly communicated with the tank body, a formaldehyde dropping port is arranged between the alkaline solution dropping port and the observation port, the formaldehyde dropping port is fixedly communicated with the tank body, a urea charging port is arranged between the flake caustic soda charging port and the feeding port, and the bottom end of the urea charging port is fixedly communicated with the tank body;
the temperature measuring device is characterized in that water outlets are oppositely arranged on two sides of the jacket barrel, the water outlets are in through connection with the jacket barrel, air outlets are formed in the top end of the jacket barrel, an end cap is arranged at one end, away from the tank body, of each air outlet, the end cap is in threaded connection with the air outlets, a water injection steam inlet is formed in the bottom end of the jacket barrel, the water injection steam inlet is in through connection with the jacket barrel, a temperature measuring sleeve is arranged on the side wall of the jacket barrel, the temperature measuring sleeve penetrates through the jacket barrel and the tank.
Further, the discharge gate has been opened at jar body bottom center, the discharge gate below is equipped with the bleeder valve, the bleeder valve top is fixed with the discharge gate and is communicate, and jar body bottom one side is fixed with the sample connection, the sample connection runs through jar body and presss from both sides the cover barrel, and the sample connection is kept away from jar body one end and is sealed with bolt threaded connection.
Further, the feed inlet top is equipped with the feed lid, and the feed lid edge is opened has a plurality of evenly distributed's U-shaped groove, and feed inlet one side is fixed with the free bearing, and feed lid edge is fixed with the hinge frame, the hinge frame is connected with the hinge bearing top hinge, and the feed inlet side is fixed with a plurality of evenly distributed's mount, install the screw rod on the mount, the screw rod bottom is connected with the mount hinge, and the screw rod cooperatees with feed lid edge U-shaped groove, and screw rod top spiro union has the nut, and the installation is fixed with the handle on the feed lid.
Furthermore, regulating valves are fixed at the top ends of the formaldehyde dropping port and the alkali solution dropping port.
Further, rabbling mechanism includes motor, speed reducer, frame, shaft coupling, (mixing) shaft, motor output and speed reducer input fixed connection, speed reducer and frame top fixed connection, frame bottom and fixing base fixed connection, shaft coupling fixed connection is passed through on the speed reducer output and the (mixing) shaft top, and the (mixing) shaft runs through fixing base and jar body, and the fixing base top is equipped with the sealing washer, and the (mixing) shaft rotates with jar body, fixing base and sealing washer respectively to be connected, and the (mixing) shaft bottom is equipped with the shaft bracket, shaft bracket bottom and the internal portion bottom fixed connection of jar, shaft bracket top are fixed with sealed bearing, and the (mixing) shaft bottom rotates with sealed bearing to be connected, and the (mixing) shaft bottom mounting has the frame agitator, frame agitator top is equipped with.
The invention has the beneficial effects that:
according to the invention, a proper amount of water is injected between the tank body and the jacket cylinder body through the water and steam injection port to serve as a heating medium, then water vapor is injected between the tank body and the jacket cylinder body from the water and steam injection port to heat the water, the water outlet is closed, the plug at the top end of the air outlet is opened to exhaust the air, and the material in the tank body is indirectly heated, so that the material in the tank body can be heated uniformly, and simultaneously, the material can be heated at a lower heating rate, the phenomenon of boiling spray kettle caused by over-fast heating of the material and delayed cooling of the reaction speed is effectively avoided;
according to the invention, circulating cooling water is injected between the tank body and the jacket barrel through the water injection and steam addition port to cool the tank body, deionized water is added into the tank body from the water inlet, the motor is started to drive the stirring shaft to rotate, the turbine stirrer and the frame stirrer rotate to fully stir and contact the deionized water and reactants, the sealing pipe connected with the water vapor outlet is opened, water vapor in the tank body is discharged in time, so that reaction heat in the tank body is led out through evaporation of the deionized water, and the danger caused by pressure rise in the tank body 1 is avoided;
according to the invention, the reaction time, the heating rate and the temperature are accurately controlled, different reaction temperatures are controlled at different reaction stages, and the tank body is cooled in time, so that the problems of overlong reaction time and overhigh reaction temperature are effectively avoided, and the viscosity of the water-based phenolic resin is moderate; and urea is added during the condensation reaction, and the urea and formaldehyde are subjected to urea-formaldehyde reaction to reduce free formaldehyde in the product, so that the formaldehyde can be effectively prevented from being gasified in the reaction temperature rise process, the product quality is improved, and the waste gas is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural view of a closed reaction vessel according to the present invention;
FIG. 2 is a top view of a closed reaction vessel according to the present invention;
FIG. 3 is a partial cross-sectional view of the invention at viewing window B-B of FIG. 2;
FIG. 4 is a schematic structural view of a feed port of the closed reaction kettle of the present invention;
fig. 5 is a partial enlarged view of the invention at a in fig. 1.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a tank body; 101. a feed inlet; 102. a fixed seat; 103. a viewing port; 104. a water vapor outlet; 105. a formaldehyde dropping port; 106. an aqueous alkali dropping port; 107. a flake caustic feeding port; 108. a urea feed port; 109. an oxalic acid feed port; 110. a water inlet; 111. a sampling port; 112. a discharge port; 113. a discharge valve; 114. a feeding cover; 115. a handle; 116. a screw; 117. a nut; 118. a fixed mount; 119. hinging seat; 120. hinging frame; 121. adjusting a valve; 2. a jacket cylinder; 201. a water outlet; 202. an air outlet; 203. a plug; 204. a water and steam injection port; 205. a temperature measuring sleeve; 3. a stirring mechanism; 301. a motor; 302. a speed reducer; 303. a frame; 304. a coupling; 305. a seal ring; 306. a stirring shaft; 307. a turbine agitator; 308. a frame-type stirrer; 309. a shaft support; 310. sealing the bearing; 4. and (4) a support.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the water-based phenolic resin comprises the following raw materials in parts by weight: 75 parts of formaldehyde solution, 30 parts of phenol, 45 parts of urea, 0.1 part of caustic soda flakes, 0.1 part of sodium hydroxide solution, 0.4 part of sodium carbonate, 2 parts of triethylamine, 1 part of N-methylethanolamine, 1 part of 2-dimethylethanolamine, 0.01 part of oxalic acid and 50 parts of deionized water.
The formaldehyde solution is 44% formaldehyde aqueous solution by mass, and the sodium hydroxide solution is 40% sodium hydroxide aqueous solution by mass.
A preparation method of water-based phenolic resin specifically comprises the following steps:
the method comprises the following steps: triethylamine, 2-dimethylethanolamine, N-methylethanolamine, phenol and sodium carbonate are added into the tank body 1 from a feed port 101 of a closed reaction kettle according to the weight part ratio, then a feed cover 114 is closed, and the feed cover 114 and the feed port 101 are locked and closed through a screw 116 and a nut 117;
step two: injecting clear water between the tank body 1 and the jacket cylinder body 2 to a water outlet 201 through a water injection and steam adding port 204, then injecting steam between the tank body 1 and the jacket cylinder body 2 through the water injection and steam adding port 204, wherein the steam firstly heats the clear water between the tank body 1 and the jacket cylinder body 2, the clear water then heats the tank body 1, the temperature in the reaction tank body 1 is controlled to be kept at 60 ℃, a sodium hydroxide solution is added into the tank body 1 from an alkaline solution dripping port 106 through a closed pipeline, a formaldehyde solution is added into the tank body 1 from a formaldehyde dripping port 105 through a closed pipeline, regulating valves 121 on the formaldehyde dripping port 105 and the alkaline solution dripping port 106 are regulated, and the dripping time of the sodium hydroxide solution and the formaldehyde solution is controlled to be 1.5 h;
step three: after the dropwise addition of the sodium hydroxide solution and the formaldehyde solution is finished, heating to 75 ℃ at the heating rate of 0.5 ℃/min, then injecting cooling water from a water injection steam inlet 204, discharging hot water from a water discharge port 201, keeping the temperature in the tank body 1 at 75 ℃, and preserving the heat for 4 hours to generate emulsion;
step four: cooling water is continuously injected from the water injection and steam injection port 204, hot water is discharged from the water discharge port 201, and when the temperature of the emulsion is reduced to 60 ℃, the flake caustic soda and the urea are respectively injected into the tank body 1 from the flake caustic soda feed port 107 and the urea feed port 108 through closed pipelines;
step five: adding oxalic acid into the tank body 1 from an oxalic acid feeding port 109 through a closed pipeline; adding deionized water into the tank body 1 from the water inlet 110 through a closed pipeline, then starting the motor 301, stirring at the rotating speed of 600r/min, and stopping stirring when the temperature in the tank body 1 is reduced to 25 ℃ to generate the water-based phenolic resin product.
Example 2:
the water-based phenolic resin comprises the following raw materials in parts by weight: 78 parts of formaldehyde solution, 31 parts of phenol, 47 parts of urea, 0.1 part of caustic soda flakes, 0.1 part of sodium hydroxide solution, 0.4 part of sodium carbonate, 2 parts of triethylamine, 1 part of N-methylethanolamine, 1 part of 2-dimethylethanolamine, 0.01 part of oxalic acid and 60 parts of deionized water.
The formaldehyde solution is 44% by mass of formaldehyde aqueous solution, and the sodium hydroxide solution is 41% by mass of sodium hydroxide aqueous solution.
A preparation method of water-based phenolic resin specifically comprises the following steps:
the method comprises the following steps: triethylamine, 2-dimethylethanolamine, N-methylethanolamine, phenol and sodium carbonate are added into the tank body 1 from a feed port 101 of a closed reaction kettle according to the weight part ratio, then a feed cover 114 is closed, and the feed cover 114 and the feed port 101 are locked and closed through a screw 116 and a nut 117;
step two: injecting clear water between the tank body 1 and the jacket cylinder body 2 to a water outlet 201 through a water injection and steam adding port 204, then injecting steam between the tank body 1 and the jacket cylinder body 2 through the water injection and steam adding port 204, wherein the steam firstly heats the clear water between the tank body 1 and the jacket cylinder body 2, the clear water then heats the tank body 1, the temperature in the reaction tank body 1 is controlled to be kept at 62 ℃, a sodium hydroxide solution is added into the tank body 1 from an alkaline solution dripping port 106 through a closed pipeline, a formaldehyde solution is added into the tank body 1 from a formaldehyde dripping port 105 through a closed pipeline, regulating valves 121 on the formaldehyde dripping port 105 and the alkaline solution dripping port 106 are regulated, and the dripping time of the sodium hydroxide solution and the formaldehyde solution is controlled to be 1.5 h;
step three: after the dropwise addition of the sodium hydroxide solution and the formaldehyde solution is finished, heating to 75 ℃ at the heating rate of 0.5 ℃/min, then injecting cooling water from a water injection steam inlet 204, discharging hot water from a water discharge port 201, keeping the temperature in the tank body 1 at 75 ℃, and preserving the heat for 4 hours to generate emulsion;
step four: cooling water is continuously injected from the water injection and steam injection port 204, hot water is discharged from the water discharge port 201, and when the temperature of the emulsion is reduced to 63 ℃, the flake caustic soda and the urea are respectively injected into the tank body 1 from the flake caustic soda feed port 107 and the urea feed port 108 through closed pipelines;
step five: adding oxalic acid into the tank body 1 from an oxalic acid feeding port 109 through a closed pipeline; adding deionized water into the tank body 1 from the water inlet 110 through a closed pipeline, then starting the motor 301, stirring at the rotating speed of 720r/min, and stopping stirring when the temperature in the tank body 1 is reduced to 25 ℃ to generate the water-based phenolic resin product.
Example 3:
the water-based phenolic resin comprises the following raw materials in parts by weight: 80 parts of formaldehyde solution, 32 parts of phenol, 50 parts of urea, 0.1 part of caustic soda flakes, 0.1 part of sodium hydroxide solution, 0.4 part of sodium carbonate, 2 parts of triethylamine, 1 part of N-methylethanolamine, 1 part of 2-dimethylethanolamine, 0.01 part of oxalic acid and 70 parts of deionized water.
The formaldehyde solution is 44% formaldehyde aqueous solution by mass, and the sodium hydroxide solution is 42% sodium hydroxide aqueous solution by mass.
A preparation method of water-based phenolic resin specifically comprises the following steps:
the method comprises the following steps: triethylamine, 2-dimethylethanolamine, N-methylethanolamine, phenol and sodium carbonate are added into the tank body 1 from a feed port 101 of a closed reaction kettle according to the weight part ratio, then a feed cover 114 is closed, and the feed cover 114 and the feed port 101 are locked and closed through a screw 116 and a nut 117;
step two: injecting clear water between the tank body 1 and the jacket cylinder body 2 to a water outlet 201 through a water injection and steam adding port 204, then injecting steam between the tank body 1 and the jacket cylinder body 2 through the water injection and steam adding port 204, wherein the steam firstly heats the clear water between the tank body 1 and the jacket cylinder body 2, the clear water then heats the tank body 1, the temperature in the reaction tank body 1 is controlled to be kept at 65 ℃, a sodium hydroxide solution is added into the tank body 1 from an alkaline solution dripping port 106 through a closed pipeline, a formaldehyde solution is added into the tank body 1 from a formaldehyde dripping port 105 through the closed pipeline, regulating valves 121 on the formaldehyde dripping port 105 and the alkaline solution dripping port 106 are regulated, and the dripping time of the sodium hydroxide solution and the formaldehyde solution is controlled to be 2 hours;
step three: after the dropwise addition of the sodium hydroxide solution and the formaldehyde solution is finished, heating to 75 ℃ at the heating rate of 0.5 ℃/min, then injecting cooling water from a water injection steam inlet 204, discharging hot water from a water discharge port 201, keeping the temperature in the tank body 1 at 75 ℃, and preserving the heat for 4 hours to generate emulsion;
step four: cooling water is continuously injected from the water injection and steam injection port 204, hot water is discharged from the water discharge port 201, and when the temperature of the emulsion is reduced to 65 ℃, the caustic soda flakes and the urea are respectively injected into the tank body 1 from the caustic soda flake feeding port 107 and the urea feeding port 108 through closed pipelines;
step five: adding oxalic acid into the tank body 1 from an oxalic acid feeding port 109 through a closed pipeline; adding deionized water into the tank body 1 from the water inlet 110 through a closed pipeline, then starting the motor 301, stirring at the rotating speed of 800r/min, and stopping stirring when the temperature in the tank body 1 is reduced to 25 ℃, thus generating the water-based phenolic resin product.
Referring to fig. 1-5, the closed reaction kettle in the above embodiment includes a tank 1, a jacket cylinder 2, a stirring mechanism 3 and a support 4, wherein the jacket cylinder 2 is sleeved at the bottom end of the outside of the tank 1, the jacket cylinder 2 is fixed to the tank 1 in a sealing manner, the stirring mechanism 3 penetrates through the top end of the tank 1, a plurality of the supports 4 are uniformly distributed on one side of the jacket cylinder 2 away from the tank 1, and the supports 4 are fixed above the side wall of the jacket cylinder 2;
a feed inlet 101 is arranged on one side of the top end of the tank body 1, the feed inlet 101 is fixedly communicated with the tank body 1, a fixed seat 102 is arranged at the center of the top end of the tank body 1, a through hole is formed in the center of the fixed seat 102 and penetrates through the top end of the tank body 1, an observation port 103 is arranged on one side, away from the feed inlet 101, of the fixed seat 102, the observation port 103 penetrates through the top end of the tank body 1 and is fixedly connected with the tank body 1, a transparent sealing plate is arranged at the center of the observation port 103, a caustic soda flake feed port 107 and a water inlet 110 are oppositely arranged on two sides of the fixed seat 102, the bottom ends of the caustic soda flake feed port 107 and the water inlet 110 are respectively and fixedly communicated with the tank body 1, a water vapor outlet 104 is arranged between the observation port 103 and the water inlet 110, the bottom end of the water vapor outlet 104 is fixedly communicated with, the alkali solution dropping port 106 is fixedly communicated with the tank body 1, a formaldehyde dropping port 105 is arranged between the alkali solution dropping port 106 and the observation port 103, the formaldehyde dropping port 105 is fixedly communicated with the tank body 1, a urea feeding port 108 is arranged between the flake alkali feeding port 107 and the feeding port 101, and the bottom end of the urea feeding port 108 is fixedly communicated with the tank body 1;
the water outlet 201 is oppositely arranged on two sides of the jacket barrel 2, the water outlet 201 is in through connection with the jacket barrel 2, the top end of the jacket barrel 2 is provided with an air outlet 202, one end, away from the tank body 1, of the air outlet 202 is provided with a plug 203, the plug 203 is in threaded connection with the air outlet 202, the bottom end of the jacket barrel 2 is provided with a water injection steam adding port 204, the water injection steam adding port 204 is in through connection with the jacket barrel 2, the side wall of the jacket barrel 2 is provided with a temperature measuring sleeve 205, the temperature measuring sleeve 205 penetrates through the jacket barrel 2 and the tank body 1, and the temperature measuring sleeve 205.
The utility model discloses a jar body 1, including jar body 1, discharge gate 112, sampling port 111, jar body 1, sampling port 111 runs through jar body 1 and cover barrel 2, and jar body 1 one end and bolt threaded connection are kept away from to sampling port 111, and the discharge gate 112 below is equipped with bleeder valve 113, the fixed intercommunication of discharge gate 113 top and discharge gate 112, jar body 1 bottom one side, sampling port 111 is fixed with sampling port 111, and it is sealed that jar body 1 one end.
Regulating valves 121 are fixed at the top ends of the formaldehyde dropping port 105 and the alkaline solution dropping port 106.
The stirring mechanism 3 comprises a motor 301, a speed reducer 302, a frame 303, a coupler 304 and a stirring shaft 306, wherein the output end of the motor 301 is fixedly connected with the input end of the speed reducer 302, the speed reducer 302 is fixedly connected with the top end of the frame 303, the bottom end of the frame 303 is fixedly connected with a fixed seat 102, the output end of the speed reducer 302 is fixedly connected with the top end of the stirring shaft 306 through the coupler 304, the stirring shaft 306 penetrates through the fixed seat 102 and the tank body 1, a sealing ring 305 is arranged above the fixed seat 102, the stirring shaft 306 is respectively and rotatably connected with the tank body 1, the fixed seat 102 and the sealing ring 305, a shaft bracket 309 is arranged at the bottom end of the stirring shaft 306, the bottom end of the shaft bracket 309 is fixedly connected with the bottom end inside the tank body 1, a sealing bearing 310 is fixed at the top end of the, the turbine stirrer 307 is fixedly connected with the stirring shaft 306.
The working principle of the invention is as follows:
under the action of triethylamine and sodium carbonate as catalysts, phenol and formaldehyde are subjected to addition reaction firstly, wherein ortho, meta and para positions of the phenol are substituted by the formaldehyde to generate hydroxymethyl phenol; reacting phenol with hydroxymethyl phenol, reacting the hydroxymethyl phenol, reacting phenol or hydroxymethyl phenol with a dimer or polymer, and reacting the polymer to finally generate the phenolic resin; adding urea and formaldehyde to perform urea-formaldehyde reaction so as to reduce free aldehyde in the product;
after raw materials are added from a feeding hole 101, a screw 116 and a nut 117 are matched with a feeding cover 114, the rest of steam outlets 104, a formaldehyde dropping hole 105, an alkali solution dropping hole 106, a flake alkali feeding hole 107, a urea feeding hole 108, an oxalic acid feeding hole 109 and a water inlet 110 are communicated with a sealed pipeline of corresponding materials, a sampling hole 111 is sealed by screwing bolts, and a discharge valve 113 below a discharge hole 112 is closed, so that the tank body 1 is in a sealed state;
when heating is needed, firstly, a proper amount of water is injected between the tank body 1 and the jacket cylinder 2 through the water and steam injection port 204 to serve as a heating medium, then, water vapor is injected between the tank body 1 and the jacket cylinder 2 from the water and steam injection port 204 to heat the water, the water outlet 201 is closed, the plug 203 at the top end of the air outlet 202 is opened to exhaust, and materials in the tank body 1 are indirectly heated, so that the materials in the tank body 1 are heated uniformly and can be heated at a lower heating rate, and the phenomenon of boiling kettle spraying caused by over-fast material heating and delayed cooling due to aggravation of reaction speed is effectively avoided;
when the temperature needs to be reduced, firstly, the air outlet 202 is sealed by the plug 203, then the water outlet 201 is opened, cooling water is injected between the tank body 1 and the jacket barrel 2 through the water injection and steam adding port 204, the tank body 1 is cooled, meanwhile, deionized water is added into the tank body 1 from the water inlet 110, the motor 301 is started, the output end of the motor 301 drives the input end of the speed reducer 302 to rotate, the output end of the speed reducer 302 drives the stirring shaft 306 to rotate through the coupler 304, the stirring shaft 306 drives the turbine stirrer 307 and the frame stirrer 308 to rotate, the deionized water is fully contacted with reactants, then, the sealing pipe connected with the water steam outlet 104 is opened, so that water steam in the tank body 1 is timely discharged, and the danger caused by;
the reaction condition in the tank body 1 can be observed in real time through the observation port 103, the reaction temperature in the tank body 1 can be monitored in real time through the temperature measuring sleeve 205, and the injection speed of cooling water is controlled through temperature change; after the reaction is finished, the product can be transferred to a storage tank or a warehouse for storage through the discharge hole 112 at the bottom of the tank body 1.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A water-based phenolic resin is characterized in that: the feed comprises the following raw materials in parts by weight: 75-80 parts of formaldehyde solution, 30-32 parts of phenol, 45-50 parts of urea, 0.1 part of caustic soda flakes, 0.1 part of sodium hydroxide solution, 0.4 part of sodium carbonate, 2 parts of triethylamine, 1 part of N-methylethanolamine, 1 part of 2-dimethylethanolamine, 0.01 part of oxalic acid and 50-70 parts of deionized water;
the water-based phenolic resin is prepared by the following steps:
the method comprises the following steps: adding triethylamine, 2-dimethylethanolamine, N-methylethanolamine, phenol and sodium carbonate into a closed reaction kettle respectively according to the weight part ratio, and then closing the closed reaction kettle;
step two: heating the closed reaction kettle, controlling the temperature in the closed reaction kettle to be kept at 60-65 ℃, adding a sodium hydroxide solution and a formaldehyde solution into the closed reaction kettle, adjusting the dropping speed of the formaldehyde solution and the sodium hydroxide solution, and controlling the dropping time of the sodium hydroxide solution and the formaldehyde solution to be 1.5-2 h;
step three: after the dropwise addition of the sodium hydroxide solution and the formaldehyde solution is finished, heating to 75 ℃ at the heating rate of 0.5 ℃/min, and preserving heat for 4 hours to generate emulsion;
step four: when the temperature of the emulsion is reduced to 60-65 ℃, putting the caustic soda flakes and the urea into a closed reaction kettle respectively through a closed pipeline;
step five: oxalic acid and deionized water are added into a closed reaction kettle from oxalic acid through a closed pipeline, stirred at the rotating speed of 600 plus 800r/min, and stopped when the temperature is reduced to 25 ℃, thus generating the water-based phenolic resin product.
2. The water-based phenolic resin according to claim 1, wherein: the formaldehyde solution is 44% formaldehyde aqueous solution, and the sodium hydroxide solution is 40-42% sodium hydroxide aqueous solution.
3. The method for preparing a water-based phenolic resin according to claim 1, wherein: the method specifically comprises the following steps:
the method comprises the following steps: triethylamine, 2-dimethylethanolamine, N-methylethanolamine, phenol and sodium carbonate are added into the tank body (1) from a feed port (101) of a closed reaction kettle according to the weight part ratio, then a feed cover (114) is closed, and the feed cover (114) and the feed port (101) are locked and closed through a screw (116) and a nut (117);
step two: injecting clear water between the tank body (1) and the jacket cylinder body (2) to a water outlet (201) through a water injection and steam adding port (204), then injecting steam between the tank body (1) and the jacket cylinder body (2) through the water injection and steam adding port (204), wherein the steam firstly heats the clear water between the tank body (1) and the jacket cylinder body (2), the clear water then heats the tank body (1), the temperature in the reverse tank body (1) is controlled to be kept at 60-65 ℃, sodium hydroxide solution is added into the tank body (1) from an aqueous alkali dropping port (106) through a closed pipeline, formaldehyde solution is added into the tank body (1) from a formaldehyde dropping port (105) through the closed pipeline, regulating valves (121) on the formaldehyde dropping port (105) and the aqueous alkali dropping port (106) are regulated, and the dropping time of the sodium hydroxide solution and the formaldehyde solution is controlled to be 1.5-2 h;
step three: after the dropwise addition of the sodium hydroxide solution and the formaldehyde solution is finished, heating to 75 ℃ at the heating rate of 0.5 ℃/min, then injecting cooling water from a water injection steam adding port (204), discharging hot water from a water discharging port (201), keeping the temperature in the tank body (1) at 75 ℃, and preserving the temperature for 4 hours to generate emulsion;
step four: cooling water is continuously injected from a water injection and steam adding port (204), hot water is discharged from a water discharge port (201), and when the temperature of the emulsion is reduced to 60-65 ℃, the caustic soda flake and the urea are respectively put into the tank body (1) from a caustic soda flake feeding port (107) and a urea feeding port (108) through closed pipelines;
step five: adding oxalic acid into the tank body (1) from an oxalic acid feeding port (109) through a closed pipeline; deionized water is added into the tank body (1) from the water inlet (110) through a closed pipeline, then the motor (301) is started to stir at the rotating speed of 600 plus 800r/min, and the stirring is stopped when the temperature in the tank body (1) is reduced to 25 ℃, so that the water-based phenolic resin product is generated.
4. The method for preparing a water-based phenolic resin according to claim 3, wherein: the closed reaction kettle comprises a tank body (1), a jacket cylinder (2), a stirring mechanism (3) and supports (4), wherein the jacket cylinder (2) is sleeved at the bottom end of the outside of the tank body (1), the jacket cylinder (2) is fixed with the tank body (1) in a sealing manner, the stirring mechanism (3) penetrates through the top end of the tank body (1), the supports (4) are uniformly distributed on one side, far away from the tank body (1), of the jacket cylinder (2), and the supports (4) are fixed above the side wall of the jacket cylinder (2);
the device is characterized in that a feed inlet (101) is arranged on one side of the top end of the tank body (1), the feed inlet (101) is fixedly communicated with the tank body (1), a fixed seat (102) is arranged at the center of the top end of the tank body (1), a through hole is formed in the center of the fixed seat (102) and penetrates through the top end of the tank body (1), an observation port (103) is arranged on one side, away from the feed inlet (101), of the fixed seat (102), the observation port (103) penetrates through the top end of the tank body (1) and is fixedly connected with the tank body (1), a transparent sealing plate is arranged at the center of the observation port (103), a caustic soda flake feed port (107) and a water inlet (110) are oppositely arranged on two sides of the fixed seat (102), the bottoms of the caustic flake feed port (107) and the water inlet (110) are respectively and fixedly communicated with the tank body (1), a water vapor, an oxalic acid feeding port (109) is arranged between the water inlet (110) and the feeding port (101), the bottom end of the oxalic acid feeding port (109) is fixedly communicated with the tank body (1), an alkali solution dropping port (106) is arranged on one side, away from the oxalic acid feeding port (109), of the fixing seat (102), the alkali solution dropping port (106) is fixedly communicated with the tank body (1), a formaldehyde dropping port (105) is arranged between the alkali solution dropping port (106) and the observation port (103), the formaldehyde dropping port (105) is fixedly communicated with the tank body (1), a urea feeding port (108) is arranged between the flake alkali feeding port (107) and the feeding port (101), and the bottom end of the urea feeding port (108) is fixedly communicated with the tank body (1);
the water and steam injection type temperature measuring device is characterized in that water outlets (201) are oppositely arranged on two sides of the jacket barrel (2), the water outlets (201) are communicated with the jacket barrel (2), air outlet holes (202) are formed in the top end of the jacket barrel (2), one end, far away from the tank body (1), of each air outlet hole (202) is provided with a plug (203), each plug (203) is in threaded connection with the corresponding air outlet hole (202), a water and steam injection port (204) is formed in the bottom end of the jacket barrel (2), the water and steam injection port (204) is communicated with the jacket barrel (2), a temperature measuring sleeve (205) is arranged on the side wall of the jacket barrel (2), the temperature measuring sleeve (205) penetrates through the jacket barrel (2) and the tank body (1), and the.
5. The method for preparing a water-based phenolic resin according to claim 4, wherein: the utility model discloses a jar body (1) is fixed with the cover barrel (2), jar body (1) bottom center is opened there is discharge gate (112), discharge gate (112) below is equipped with bleeder valve (113), bleeder valve (113) top and discharge gate (112) fixed intercommunication, jar body (1) bottom one side is fixed with sample connection (111), sample connection (111) run through jar body (1) and press from both sides cover barrel (2), and sample connection (111) are kept away from jar body (1) one end and is sealed with bolt threaded connection.
6. The method for preparing a water-based phenolic resin according to claim 4, wherein: feed inlet (101) top is equipped with feed cover (114), and feed cover (114) edge is opened has a plurality of evenly distributed's U-shaped groove, and feed inlet (101) one side is fixed with free bearing (119), and feed cover (114) edge is fixed with hinge frame (120), hinge frame (120) are connected with hinge bearing (119) top hinge, and feed inlet (101) side is fixed with a plurality of evenly distributed's mount (118), install screw rod (116) on mount (118), screw rod (116) bottom and mount (118) hinge, screw rod (116) and feed cover (114) edge U-shaped groove cooperate, and screw rod (116) top spiro union has nut (117), and the installation is fixed with handle (115) on feed cover (114).
7. The method for preparing a water-based phenolic resin according to claim 4, wherein: regulating valves (121) are fixed at the top ends of the formaldehyde dropping port (105) and the alkali solution dropping port (106).
8. The method for preparing a water-based phenolic resin according to claim 4, wherein: the stirring mechanism (3) comprises a motor (301), a speed reducer (302), a rack (303), a coupler (304) and a stirring shaft (306), the output end of the motor (301) is fixedly connected with the input end of the speed reducer (302), the speed reducer (302) is fixedly connected with the top end of the rack (303), the bottom end of the rack (303) is fixedly connected with a fixed seat (102), the output end of the speed reducer (302) is fixedly connected with the top end of the stirring shaft (306) through the coupler (304), the stirring shaft (306) penetrates through the fixed seat (102) and the tank body (1), a sealing ring (305) is arranged above the fixed seat (102), the stirring shaft (306) is respectively rotatably connected with the tank body (1), the fixed seat (102) and the sealing ring (305), a shaft support (309) is arranged at the bottom end of the stirring shaft (306), the bottom end of the shaft support (309) is fixedly connected with, the bottom end of the stirring shaft (306) is rotatably connected with the sealing bearing (310), a frame stirrer (308) is fixed at the bottom end of the stirring shaft (306), a turbine stirrer (307) is arranged above the frame stirrer (308), and the turbine stirrer (307) is fixedly connected with the stirring shaft (306).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113831490A (en) * | 2021-09-17 | 2021-12-24 | 安徽弘源化工科技有限公司 | High-strength water-based phenolic resin and preparation method thereof |
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