CN106753176A - A kind of aqueous polyurethane cardboard adhesive of Antimicrobial preservative excellent performance and preparation method thereof - Google Patents
A kind of aqueous polyurethane cardboard adhesive of Antimicrobial preservative excellent performance and preparation method thereof Download PDFInfo
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- CN106753176A CN106753176A CN201611205051.3A CN201611205051A CN106753176A CN 106753176 A CN106753176 A CN 106753176A CN 201611205051 A CN201611205051 A CN 201611205051A CN 106753176 A CN106753176 A CN 106753176A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6492—Lignin containing materials; Wood resins; Wood tars; Derivatives thereof
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/6541—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/34
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C08G2170/00—Compositions for adhesives
- C08G2170/80—Compositions for aqueous adhesives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Paper (AREA)
Abstract
The present invention discloses a kind of aqueous polyurethane cardboard adhesive of Antimicrobial preservative excellent performance, is made up of the raw material of following weight portion：Polyethylene glycol 45 60, dicyclohexyl methyl hydride diisocyanate 25 35, raw alkaline lignin 4 10,10% NaOH solution is appropriate, 10% hydrochloric acid solution is appropriate, IPDI 8 15, dibutyl tin laurate 0.4 0.8, acetone in proper, diethanol amine 10 25, tung oil 5 12, caustic alcohol 0.4 0.8, dihydromethyl propionic acid 38, N methyl pyrrolidones are appropriate, N methyl diethanolamines 39, triethylamine 15 25, rosin resin emulsion 14, distillation appropriate amount of water, nano silicon micronization 58, sodium sulfanilate 12, rosin 13.The present invention introduces the lignin modified through NCO group in Aqueous Polyurethane Adhesives, increases bonding force of the adhesive to paper, another water resistance that can improve Aqueous Polyurethane Adhesives, and product has the features such as adhesive fastness is good, nothing is gone rotten.
Description
Technical field
It is exactly a kind of aqueous polyurethane cardboard glue of Antimicrobial preservative excellent performance the present invention relates to adhesive field
Glutinous agent and preparation method thereof.
Background technology
The bonding of object, realizes, the solvent in glue carries macromolecule by the pulling force between the polymer body in glue
Body is immersed in the tissue of object at leisure, and after disappearing solvent in glue, the polymer body in glue is just by mutual
Pulling force, by the combination tightly of two objects, existing paper adhesives are many to have the phenomenon, particularly shadow such as get damp, go rotten
Ring the feel of paper and there is serious environmental issue.
Adhesive for polyurethane has the performances such as soft durometer, and controllability is good, low temperature resistant, and pliability is good, and adhesive strength is big etc.
Advantage, but, at present in whole adhesive for polyurethane field based on solvent borne polyurethane adhesive, it has the disadvantage organic molten
Agent smell is big, volatile, caused when using air pollution, it is inflammable, more or less there is toxicity etc., therefore the poly- ammonia in various countries in recent years
Ester material researcher takes quite some effort the R and D for carrying out Aqueous Polyurethane Adhesives.Aqueous polyurethane is one
Plant the binary colloidal system that polyurethane particles are dispersed in water.Aqueous polyurethane with water as medium, with safety, do not burn, nothing
The particular advantages of public hazards.
Liu Lu, Ren Zhiyong et al. are at it《The preparation of amphotenic polkyurethanes aqueous dispersion and performance are ground derived from hydroxylated tung oil
Study carefully》In one text, with polyethylene glycol（PEG-800）, N methyldiethanol amine（MDEA）, dihydromethyl propionic acid（DMPA）, 4,4'- bis-
Diphenylmethane diisocyanate（HMDI）And hydroxylated tung oil（HTO）Deng being raw material, synthesize two derived from hydroxylated tung oil
Property polyurethane（HTO-ZPUD）, the water resistance and solvent resistance of aqueous amphotenic polkyurethanes are improved by post-crosslinking, but its viscosity is not
Foot.
Therefore, the present invention introduces the lignin of warp-NCO group modification in Aqueous Polyurethane Adhesives, increases adhesive
To the bonding force of paper, another water resistance that can improve Aqueous Polyurethane Adhesives.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of aqueous poly- ammonia of Antimicrobial preservative excellent performance
Ester cardboard adhesive and preparation method thereof.
A kind of aqueous polyurethane cardboard adhesive of Antimicrobial preservative excellent performance, is made up of the raw material of following weight portion：It is poly-
Ethylene glycol 45-60 parts, dicyclohexyl methyl hydride diisocyanate 25-35 parts, raw alkaline lignin 4-10 parts, 10% NaOH solution is fitted
Amount, 10% hydrochloric acid solution is appropriate, IPDI 8-15 parts, dibutyl tin laurate 0.4-0.8 parts, and acetone is fitted
Amount, diethanol amine 10-25 parts, tung oil 5-12 parts, caustic alcohol 0.4-0.8 parts, dihydromethyl propionic acid 3-8 parts, N- crassitudes
Appropriate ketone, N methyldiethanol amine 3-9 parts, triethylamine 15-25 parts, 1-4 parts of rosin resin emulsion distills appropriate amount of water, nano-silicon
Micro mist 5-8 parts, sodium sulfanilate 1-2 parts, rosin 1-3 parts.
Comprise the following steps that：
（1）The preparation of-NCO sill quality：
1. raw alkaline lignin, is configured to the aqueous solution that concentration is 30%, with mass fraction be 10% NaOH solution adjust pH to
13-14, makes alkali lignin that insoluble matter is removed after fully dissolving, and then lowers pH to 2-3 in 55-65 DEG C with 10% hydrochloric acid solution, sinks
Form sediment alkali lignin, filtering, is precipitated to neutrality with distillation water washing repeatedly, in 50-70 DEG C of vacuum drying, obtains alkali lignin standby
With；
2., in the single port bottle whisked with magnetic force add IPDI, dibutyl tin laurate, acetone and
Above-mentioned alkali lignin, after being sufficiently stirred for, 30-50 DEG C ultrasonic disperse 1-3 hours, it is then small in 50-60 DEG C of back flow reaction 3-5
When, room temperature is cooled to, at 70-85 DEG C be vacuum dried 3-4 hours filter cake by separation, acetone washing, and-NCO is obtained after grinding
Sill quality；
（2）The preparation of hydroxylated tung oil：
Tung oil and diethanol amine are added and is equipped with the four-hole boiling flask of agitator, reflux condensing tube, thermometer and nitrogen protection, in
Caustic alcohol is added at 40-55 DEG C, controlling reaction temperature is refluxed 2-5 hours between 105-125 DEG C afterwards, obtains hydroxyl
Change tung oil；
（3）The preparation of hydroxylated tung oil modified aqueous polyurethane/lignin complex emulsions：
Polyethylene glycol is placed in four-hole boiling flask 110-130 DEG C of intensification dehydrated under vacuum 2-3 hours, is cooled in a nitrogen environment
50-70 DEG C, add dicyclohexyl methyl hydride diisocyanate, step（1）- NCO sills quality stirring reaction 0.5-2 hours, is added dropwise
Dissolved with the 1-METHYLPYRROLIDONE solution of dihydromethyl propionic acid, stirring reaction 50-70 minutes at 75-85 DEG C, cooling exists temperature control
70-80 DEG C, add step（2）Hydroxylated tung oil and N methyldiethanol amine, react 1-2 hour, addition triethylamine in and 15-25
Minute, the 70-90 DEG C of emulsification that adds water is heated to, obtain hydroxylated tung oil modified aqueous polyurethane/lignin complex emulsions；
（4）Nano silicon micronization is added to 4-6 times of distilled water, sodium sulfanilate, rosin is added, is 25-35 in temperature
Under conditions of DEG C, ultrasonic disperse 15-30 minutes, mixed liquor is obtained standby；
（5）By step（3）Complex emulsions add rosin resin emulsion, shepardite and step（4）Mixed liquor, is evacuated to vacuum
It is 0.5-0.8MPa to spend, and is mixed 20-30 minutes with the speed high-speed stirred of 300-500r/min, obtains the water-borne polyurethane bond
Glutinous agent.
Compared with prior art, the present invention has advantages below：
（1）Lignin is a kind of complicated poly- aldehydes matter with three-dimensional netted stereochemical structure, and abundant alcohol is contained in molecule
Hydroxyl and phenolic hydroxyl group isoreactivity group, are reacted using these active groups in the present invention with isocyanates, obtain surface by-NCO
The lignin of base group modification, the synthetic reaction that aqueous polyurethane is participated in afterwards obtains biomass-based aqueous polyurethane emulsion, can be with
Hydroxyl in paper chemically reacts, so as to produce good bond effect, adhesive biodegradability, ring can be assigned again
Guarantor's effect is good, and the lignin of in addition-NCO group modification can react with polyethylene glycol, hydroxylated tung oil so that between segment
Interaction enhanced, lift cross-link intensity, water resistance is improved, and is not got damp after packing box bonding, without going rotten, and does not influence paper
Open feel.
（2）Hydroxylated tung oil can be regarded as containing three hydrophobic branch chains long of conjugated double bond, and being introduced into polyurethane turns into containing double
Key tung oil aqueous polyurethane emulsion, its essence is to being introduced in polyurethane containing double bond hydrophobic branch chain long so that hydrophobic association is made
With obvious, the thickening property to adhesive is better, and the Aqueous Polyurethane Adhesives of preparation have initial viscosity good, and adhesive strength is high etc.
Feature, while the introducing of double bond can improve the crosslink density of colloid, is obviously improved water-fast, the solvent resistance of product.
（3）Nano silicon micronization is added according to the antibacterial characteristics of rosin, in the present invention to adsorb rosin, rosin is uniform
Be dispersed in Aqueous Polyurethane Adhesives, make adhesive of the invention that there is excellent antibiotic property, in use can antibacterial prevent
It is mould, it is to avoid a large amount of growths of mould.
Specific embodiment
A kind of aqueous polyurethane cardboard adhesive of Antimicrobial preservative excellent performance, is made up of the raw material of following weight portion：It is poly-
Ethylene glycol 55, dicyclohexyl methyl hydride diisocyanate 28, raw alkaline lignin 8,10% NaOH solution is appropriate, and 10% hydrochloric acid solution is fitted
Amount, IPDI 12, dibutyl tin laurate 0.5, acetone in proper, diethanol amine 21, tung oil 9, caustic alcohol
0.7, dihydromethyl propionic acid 6, appropriate 1-METHYLPYRROLIDONE, N methyldiethanol amine 7, triethylamine 20, rosin resin emulsion 3,
Distillation appropriate amount of water, nano silicon micronization 7, sodium sulfanilate 1, rosin 2.
Comprise the following steps that：
（1）The preparation of-NCO sill quality：
1. raw alkaline lignin, is configured to the aqueous solution that concentration is 30%, with mass fraction be 10% NaOH solution adjust pH to
13-14, makes alkali lignin that insoluble matter is removed after fully dissolving, and pH to 2-3, precipitation are then lowered in 60 DEG C with 10% hydrochloric acid solution
Go out alkali lignin, filter, be precipitated to neutrality with distillation water washing repeatedly, in 65 DEG C of vacuum drying, obtain alkali lignin standby；
2., in the single port bottle whisked with magnetic force add IPDI, dibutyl tin laurate, acetone and
Above-mentioned alkali lignin, after being sufficiently stirred for, in 40 DEG C of ultrasonic disperses 2 hours, then in 55 DEG C of back flow reactions 4 hours, is cooled to room
Temperature, separation, acetone washing, filter cake is vacuum dried 4 hours at 80 DEG C, and-NCO sill quality is obtained after grinding；
（2）The preparation of hydroxylated tung oil：
Tung oil and diethanol amine are added and is equipped with the four-hole boiling flask of agitator, reflux condensing tube, thermometer and nitrogen protection, in
Caustic alcohol is added at 50 DEG C, controlling reaction temperature is refluxed 4 hours between 115 DEG C afterwards, obtains hydroxylated tung oil；
（3）The preparation of hydroxylated tung oil modified aqueous polyurethane/lignin complex emulsions：
Polyethylene glycol is placed in 120 DEG C of intensification dehydrated under vacuum 3 hours in four-hole boiling flask, 60 DEG C is cooled in a nitrogen environment,
Add dicyclohexyl methyl hydride diisocyanate, step（1）- NCO sill quality stirring reaction 1 hour, is added dropwise dissolved with dihydroxymethyl
The 1-METHYLPYRROLIDONE solution of propionic acid, temperature control stirring reaction 60 minutes at 80 DEG C lower the temperature at 75 DEG C, add step（2）Hydroxyl
Base tung oil and N methyldiethanol amine, react 1.5 hours, with 20 minutes in addition triethylamine, are heated to 80 DEG C of emulsifications that add water,
Obtain hydroxylated tung oil modified aqueous polyurethane/lignin complex emulsions；
（4）Nano silicon micronization is added to 5 times of distilled water, sodium sulfanilate, rosin is added, in the bar that temperature is 30 DEG C
Under part, ultrasonic disperse 25 minutes obtains mixed liquor standby；
（5）By step（3）Complex emulsions add rosin resin emulsion, shepardite and step（4）Mixed liquor, is evacuated to vacuum
It is 0.7MPa to spend, and is mixed 25 minutes with the speed high-speed stirred of 400r/min, obtains the Aqueous Polyurethane Adhesives.
The Aqueous Polyurethane Adhesives of the preparation prepared according to specific embodiment, performance test is carried out to it, as a result as follows：
The adhesive solidification time（30℃）：<50min, peel strength：105N/ (2.5cm), initial viscosity（25℃）：10290
mPa·s。
Claims (2)
1. the aqueous polyurethane cardboard adhesive of a kind of Antimicrobial preservative excellent performance, it is characterised in that by the original of following weight portion
Material composition：Polyethylene glycol 45-60 parts, dicyclohexyl methyl hydride diisocyanate 25-35 parts, raw alkaline lignin 4-10 parts, 10%
Appropriate NaOH solution, 10% hydrochloric acid solution is appropriate, IPDI 8-15 parts, dibutyl tin laurate 0.4-0.8
Part, acetone in proper, diethanol amine 10-25 parts, tung oil 5-12 parts, caustic alcohol 0.4-0.8 parts, dihydromethyl propionic acid 3-8 parts, N- first
Base pyrrolidones is appropriate, N methyldiethanol amine 3-9 parts, triethylamine 15-25 parts, 1-4 parts of rosin resin emulsion, and distilled water is fitted
Amount, nano silicon micronization 5-8 parts, sodium sulfanilate 1-2 parts, rosin 1-3 parts.
2. the preparation side of the aqueous polyurethane cardboard adhesive of a kind of Antimicrobial preservative excellent performance according to claims 1
Method, it is characterised in that comprise the following steps that：
（1）The preparation of-NCO sill quality：
1. raw alkaline lignin, is configured to the aqueous solution that concentration is 30%, with mass fraction be 10% NaOH solution adjust pH to
13-14, makes alkali lignin that insoluble matter is removed after fully dissolving, and then lowers pH to 2-3 in 55-65 DEG C with 10% hydrochloric acid solution, sinks
Form sediment alkali lignin, filtering, is precipitated to neutrality with distillation water washing repeatedly, in 50-70 DEG C of vacuum drying, obtains alkali lignin standby
With；
2., in the single port bottle whisked with magnetic force add IPDI, dibutyl tin laurate, acetone and
Above-mentioned alkali lignin, after being sufficiently stirred for, 30-50 DEG C ultrasonic disperse 1-3 hours, it is then small in 50-60 DEG C of back flow reaction 3-5
When, room temperature is cooled to, at 70-85 DEG C be vacuum dried 3-4 hours filter cake by separation, acetone washing, and-NCO is obtained after grinding
Sill quality；
（2）The preparation of hydroxylated tung oil：
Tung oil and diethanol amine are added and is equipped with the four-hole boiling flask of agitator, reflux condensing tube, thermometer and nitrogen protection, in
Caustic alcohol is added at 40-55 DEG C, controlling reaction temperature is refluxed 2-5 hours between 105-125 DEG C afterwards, obtains hydroxyl
Change tung oil；
（3）The preparation of hydroxylated tung oil modified aqueous polyurethane/lignin complex emulsions：
Polyethylene glycol is placed in four-hole boiling flask 110-130 DEG C of intensification dehydrated under vacuum 2-3 hours, is cooled in a nitrogen environment
50-70 DEG C, add dicyclohexyl methyl hydride diisocyanate, step（1）- NCO sills quality stirring reaction 0.5-2 hours, is added dropwise
Dissolved with the 1-METHYLPYRROLIDONE solution of dihydromethyl propionic acid, stirring reaction 50-70 minutes at 75-85 DEG C, cooling exists temperature control
70-80 DEG C, add step（2）Hydroxylated tung oil and N methyldiethanol amine, react 1-2 hour, addition triethylamine in and 15-25
Minute, the 70-90 DEG C of emulsification that adds water is heated to, obtain hydroxylated tung oil modified aqueous polyurethane/lignin complex emulsions；
（4）Nano silicon micronization is added to 4-6 times of distilled water, sodium sulfanilate, rosin is added, is 25-35 in temperature
Under conditions of DEG C, ultrasonic disperse 15-30 minutes, mixed liquor is obtained standby；
（5）By step（3）Complex emulsions add rosin resin emulsion, shepardite and step（4）Mixed liquor, is evacuated to vacuum
It is 0.5-0.8MPa to spend, and is mixed 20-30 minutes with the speed high-speed stirred of 300-500r/min, obtains the water-borne polyurethane bond
Glutinous agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531113A (en) * | 2018-04-20 | 2018-09-14 | 张剑 | A kind of preparation method of paper product Aqueous Adhesives |
| CN112300354A (en) * | 2019-07-31 | 2021-02-02 | 中国石油化工股份有限公司 | Lignin-based polyurethane film and synthetic method thereof |
| CN113527611A (en) * | 2021-07-29 | 2021-10-22 | 华南理工大学 | Polyurethane dispersion liquid and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845367A (en) * | 2009-07-01 | 2010-09-29 | 河南省科学院高新技术研究中心 | Hydroxylated tung oil and ester group-aminated preparation method thereof |
| CN101974305A (en) * | 2010-09-21 | 2011-02-16 | 华南理工大学 | Method for preparing waterborne polyurethane adhesive used for compound soft packaging |
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| CN112300354B (en) * | 2019-07-31 | 2022-06-07 | 中国石油化工股份有限公司 | Lignin-based polyurethane film and synthetic method thereof |
| CN113527611A (en) * | 2021-07-29 | 2021-10-22 | 华南理工大学 | Polyurethane dispersion liquid and preparation method and application thereof |
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