CN108192051A - A kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive - Google Patents
A kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive Download PDFInfo
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- CN108192051A CN108192051A CN201711303500.2A CN201711303500A CN108192051A CN 108192051 A CN108192051 A CN 108192051A CN 201711303500 A CN201711303500 A CN 201711303500A CN 108192051 A CN108192051 A CN 108192051A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- 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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/10—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to inorganic materials
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Abstract
The present invention relates to adhesive preparing technical fields, and in particular to a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive.Orthosilicic acid is generated nano silicon dioxide by thermal decomposition and is surface modified through silane coupling agent the present invention under the high temperature conditions first, then cause system by chain tra nsfer under the action of initiator to generate free radicals, and pass through group transfer reaction, generate nano silicon dioxide free radical, final nano silicon dioxide free radical can be captured by unsaturated cationic monomer, cation nanometer silica of the generation with positive charge, then by cation nanometer silica and wood tar, starch and microorganism blending fermentation, pass through microbial degradation first, generate the ester group of a large amount of free properties, hydroxyl and other chemical active radicals, and these groups are introduced into cation nanometer silica surface, tea polyphenols and xanthans blending fermentation are obtained into mixed liquor again, last and mixed liquor and acrylic monomer blending, polymerization obtains Laminating adhesive.
Description
Technical field
The present invention relates to adhesive preparing technical fields, and in particular to a kind of preparation side of water-fast high viscosity paper-plastic lamination adhesive
Method.
Background technology
Paper-plastic stick is to utilize adhesive by polypropylene（Abbreviation BOPP）Or terylene（PET）Film is answered with paper printed matter
The advantages of being combined, combining paper and plastics, so as to make printed matter surface brighter smooth, make color and luster more bright-coloured and
Rich in three-dimensional sense, while the effects that moisture-proof, antifouling, anti-fake, folding is wear-resisting is also acted as, be widely used in decorative building material, packing timber
Material, hard-cover books, products propaganda advertisement or specification etc..With the development of market economy, the raising of the level of consumption, overlay film is suitable
Extensively.
Adhesive used in paper-plastic stick is known as paper-plastic stick adhesive, abbreviation paper-plastic lamination adhesive.In recent years, it obtained
It widely applies and rapidly develops, demand also increases severely therewith.Paper-plastic lamination adhesive had both required the plastics to nonpolarity, low-surface-energy
The bonding force that film surface has had also requires the cohesive force having had to the paper surface of polarity；It is and also necessary to ink
The affinity having had, this just proposes paper-plastic lamination adhesive some particular/special requirements.
Since esters of acrylic acid adhesive contains the functional groups such as ester group, hydroxyl and carboxyl, acrylic emulsion adhesive
With very strong polarity, so adhesive property is good, the emulsion-type glue majority used in paper-plastic lamination is acrylate copolymer.By
In aqueous adhesive using water as decentralized medium, viscosity does not increase significantly with the increase of polymer molecular weight, so can be made high
Solid content, high molecular weight, high-adhesive-strength polymer, and also have many advantages, such as inexpensive, safe and environment-friendly, easy to clean.Together
When, aqueous laminating adhesive may be directly applied to existing dry complex equipment, and the performance of product can reach solvent type and answer substantially
The level of film glue has large development potentiality.The raw material of aqueous acrylic emulsion adhesive is cheap and is easy to get, production technology letter
Just, the ageing-resistant performance of product, guarantor's light protect color and excellent in mechanical performance, and the scope of application is wider, and development is very swift and violent.It does not look over so as to check
Preceding water-and acrylate emulsion adhesive there is also some problems, such as：Poor water resistance, peel strength are relatively low, bond strength
It is relatively low, the problems such as mechanical stability is poor.
Therefore, inventing a kind of property Novel paper-plastic Laminating adhesive of water-fast high viscosity has actively adhesive preparing technical field
Meaning.
Invention content
Present invention mainly solves the technical issues of, for common current water-and acrylate lotion paper-plastic lamination adhesive at present
There are poor water resistance, bond strength is relatively low, mechanical stability is poor the problem of, provide a kind of water-fast high viscosity paper-plastic lamination adhesive
Preparation method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive, it is characterised in that specifically preparation process is：
（1）It is put into reaction kettle after orthosilicic acid and water and Silane coupling agent KH550 are mixed, seals heat temperature raising in reaction kettle
It to 150~160 DEG C, is filtered after being stirred to react 1~2h, isolated filter residue；
（2）After above-mentioned filter residue and vinylbenzyltrimethyl ammonium chloride and water are mixed, mixed liquor is obtained, mixed liquor is packed into
In reaction kettle, then hydrogen peroxide and solution of ferrous chloride and benzoyl peroxide are added in into reaction kettle, sealing reaction kettle heating
100~120 DEG C are warming up to, is separated by filtration to obtain filter cake after being stirred to react 1~2h, as cation modified nano silicon dioxide；
（3）Count in parts by weight, weigh 40~50 parts of above-mentioned cation modified nano silicon dioxides, 15~20 parts of wood tar, 5~
10 parts of starch and 15~20 parts a concentration of 107The Ruminococcus albus bacteria suspension of cfu/mL is fitted into fermentation tank, is sealed by fermentation, hair
It is separated by filtration to obtain fermentation filter residue after ferment, nano silicon dioxide is modified up to modified cation after sterilizing；
（4）By tea polyphenols and biogas slurry by mass ratioes blending is waited, sealing and standing 5~7 days in insulating box are placed on, filtrate is obtained by filtration,
Xanthans and filtrate are blended again, continues to be put into sealing and standing 1~2 day in insulating box, obtains mixed liquor, mixed liquor high temperature is gone out
Bacterium obtains sterilizing mixed liquor；
（5）It counts in parts by weight, 1~2 part of OP-10,0.5~0.8 part of SE-10,1~3 part of bicarbonate is added in into three-necked flask
Sodium and 100~150 parts of water, 10~15min of stirring and dissolving obtains mixed solution, then 10~15 parts of acetic acid are added in into three-necked flask
Vinyl acetate, 8~10 parts of butyl acrylates, 12~15 parts of hydroxy-ethyl acrylates, 9~12 parts of acrylic acid, are stirred 10~15min
Obtain prefabricated solution；
（6）Above-mentioned three-necked flask is moved into water-bath, is heated to 70~80 DEG C, with constant pressure funnel to three-necked flask
Middle dropwise addition ammonium persulfate solution, control drop rate make ammonium persulfate solution be added dropwise in 25~30min, and insulated and stirred is anti-
85~95 DEG C are warming up to after answering 2~4h, continues to be stirred to react 20~30min, it is water-fast high viscosity paper that discharging, which obtains reaction solution,
Mould Laminating adhesive.
Step（1）Described in orthosilicic acid and water and Silane coupling agent KH550 be 1 in mass ratio:5:1.
Step（2）Described in filter residue and the mass ratio of vinylbenzyltrimethyl ammonium chloride and water be 4:1:38, it is double
The addition of oxygen water is the 40% of mixed liquor quality, and a concentration of 50mmol/L of hydrogen peroxide, the addition of solution of ferrous chloride is mixed
The 5% of liquid quality is closed, a concentration of 0.1mol/L of solution of ferrous chloride, the addition of benzoyl peroxide is mixed liquor quality
1%。
Step（3）Described in sealing and fermenting temperature for 25~30 DEG C, the time of sealing and fermenting is 7~9 days.
Step（4）Described in insulating box temperature for 30~40 DEG C, the mass ratio of xanthans and filtrate is 1:3, high temperature
The temperature of sterilizing is 120 DEG C, and the time of high-temperature sterilization is 10~15min.
Step（6）Described in ammonium persulfate solution dripping quantity be prefabricated solution quality 10%, the matter of ammonium persulfate solution
It is 5% to measure score.
The beneficial effects of the invention are as follows：
（1）Orthosilicic acid and silane coupling agent are blended first by the present invention, and orthosilicic acid is generated nanometer by thermal decomposition under the high temperature conditions
Silica is simultaneously surface modified through silane coupling agent, is obtained the nano silicon dioxide rich in active function groups, is then being drawn
Unsaturated cationic monomer quaternary ammonium salt is connected to nano-silica surface by Raolical polymerizable under the action of hair agent,
Cause system by chain tra nsfer to generate free radicals, and pass through group transfer reaction, generate nano silicon dioxide free radical, final nanometer
Silica free radical can be captured by unsaturated cationic monomer, cation nanometer silica of the generation with positive charge, with
Afterwards by cation nanometer silica and wood tar, starch and microorganism blending fermentation, first by microorganism by wood tar
With the starch degradation of polyhydroxy, the ester group, hydroxyl and other chemical active radicals of a large amount of free properties are generated, and passes through microorganism
These groups are introduced into cation nanometer silica surface, obtain the cation nanometer silica of polyfunctional group modification,
Again by tea polyphenols and xanthans blending fermentation obtain mixed liquor, finally by polyfunctional group modification cation nanometer silica and
Mixed liquor and acrylic monomer blending, polymerize under the action of auxiliary agent and obtain Laminating adhesive, wherein cation nanometer titanium dioxide
On the one hand the addition of silicon can improve the viscosity of Laminating adhesive, on the other hand positively charged cation nanometer silica can be with
Charge attraction power is generated between the negatively charged paper fibre in surface, so as to improve the adhesion strength of Laminating adhesive, and nanometer
Silica is immersed in glue in paper fibre, can be played the role of filling after curing and be reinforced so that its is mechanically stable
Property be also improved, the glue after curing is bonded strong by intermolecular hydrogen bond and the anchorage effect between paper fibre
Degree is further enhanced；
（2）The present invention introduces hydrophobicity ester group, ester group by modified cation nanometer silica surface
Introducing so that the water resistance of Laminating adhesive is significantly improved, the hydroxyl in addition introduced is a kind of polar group, it can be improved
Adhesion strength between Laminating adhesive and the paper fibre of polarity, and the xanthans that the present invention adds is similar due to having with fiber
Skeleton structure, thus it is preferable with the compatibility of paper fibre, itself and tea polyphenols blending fermentation are dropped tea polyphenols using microorganism
Solution generates nonpolar rigid benzene radicals, this is again so that the adhesion strength between Laminating adhesive and nonpolar thin polymer film obtains
To improve, and it polymerize between the polymerizable functional group and acrylic monomer of final nano-silica surface modification, obtains
Laminating adhesive, wherein the polyacrylate after polymerization and being expanded by molecule between viscous polymer film with similar chemical properties
It dissipates and generates cohesive force so that the adhesion strength between Laminating adhesive and polarity paper and non-polar polymer film is made in the present invention
It is all improved, water resistance and mechanical stability also significantly improve, and have broad application prospects.
Specific embodiment
It is 1 in mass ratio:5:1 will be put into after orthosilicic acid and the mixing of water and Silane coupling agent KH550 in reaction kettle, seal
150~160 DEG C are heated in reaction kettle, starts blender, after being stirred to react 1~2h with the rotating speed of 200~300r/min
Filtering, isolated filter residue；It is 4 in mass ratio by filter residue and vinylbenzyltrimethyl ammonium chloride and water:1:After 38 mixing,
Mixed liquor is obtained, mixed liquor is fitted into reaction kettle, then a concentration of 50mmol/L of mixed liquor quality 40% is added in into reaction kettle
The benzoyl peroxide of the solution of ferrous chloride and mixed liquor quality 1% of hydrogen peroxide and a concentration of 0.1mol/L of mixed liquor quality 5%
Formyl, sealing reaction kettle be heated to 100~120 DEG C, be separated by filtration to obtain filter cake after being stirred to react 1~2h, as sun from
Son modification nano silicon dioxide；It counts in parts by weight, weighs 40~50 parts of cation modified nano silicon dioxides, 15~20 parts of wood
Tar, 5~10 parts of starch and 15~20 parts a concentration of 107The Ruminococcus albus bacteria suspension of cfu/mL is fitted into fermentation tank, close
Sealed cans mouth is sealed by fermentation 7~9 days at 25~30 DEG C, is separated by filtration to obtain fermentation filter residue after fermentation, be changed to obtain the final product after sterilizing
The cation modified nano silicon dioxide of property；By tea polyphenols and biogas slurry by mass ratioes blending is waited, it is placed on the perseverance that temperature is 30~40 DEG C
Filtrate is obtained by filtration in sealing and standing 5~7 days in incubator, then is 1 in mass ratio:3 xanthans and filtrate are blended, and continue to be put into
Sealing and standing 1~2 day, obtains mixed liquor, by mixed liquor high-temperature sterilization box with 120 DEG C in the insulating box that temperature is 30~40 DEG C
Temperature sterilize 10~15min, obtain sterilizing mixed liquor；It counts in parts by weight, 1~2 part of OP-10 is added in into three-necked flask,
0.5~0.8 part of SE-10,1~3 part of sodium bicarbonate and 100~150 parts of water, 10~15min of stirring and dissolving obtain mixed solution, then
Into three-necked flask add in 10~15 parts of vinyl acetates, 8~10 parts of butyl acrylates, 12~15 parts of hydroxy-ethyl acrylates, 9~
12 parts of acrylic acid, are stirred 10~15min and obtain prefabricated solution；Three-necked flask is moved into water-bath, it is heated to 70~
80 DEG C, the mass fraction that prefabricated solution quality 10% is added dropwise into three-necked flask with constant pressure funnel is 5% ammonium persulfate solution, is controlled
Drop rate processed makes ammonium persulfate solution be added dropwise in 25~30min, and insulated and stirred is warming up to 85~95 after reacting 2~4h
DEG C, continue to be stirred to react 20~30min, it is water-fast high viscosity paper-plastic lamination adhesive that discharging, which obtains reaction solution,.
Example 1
It is 1 in mass ratio:5:1 will be put into after orthosilicic acid and the mixing of water and Silane coupling agent KH550 in reaction kettle, sealing reaction
150 DEG C are heated in kettle, starts blender, is filtered after being stirred to react 1h with the rotating speed of 200r/min, isolated filter residue；
It is 4 in mass ratio by filter residue and vinylbenzyltrimethyl ammonium chloride and water:1:After 38 mixing, mixed liquor is obtained, will be mixed
Liquid is fitted into reaction kettle, then a concentration of 50mmol/L hydrogen peroxide of mixed liquor quality 40% and mixed liquor matter are added in into reaction kettle
The solution of ferrous chloride of a concentration of 0.1mol/L of amount 5% and the benzoyl peroxide of mixed liquor quality 1%, sealing reaction kettle add
Heat is warming up to 100 DEG C, is separated by filtration to obtain filter cake after being stirred to react 1h, as cation modified nano silicon dioxide；By weight
Number meter weighs 40 parts of cation modified nano silicon dioxides, 15 parts of wood tar, 5 parts of starch and 15 parts a concentration of 107cfu/mL
Ruminococcus albus bacteria suspension be fitted into fermentation tank, sealing tank mouth is sealed by fermentation 7 days at 25 DEG C, and filtering after fermentation divides
From fermentation filter residue is obtained, nano silicon dioxide is modified up to modified cation after sterilizing；Tea polyphenols and biogas slurry are pressed and wait mass ratioes
Blending is placed on sealing and standing 5 days in the insulating box that temperature is 30 DEG C, filtrate is obtained by filtration, then is 1 in mass ratio:3 by xanthans
It is blended with filtrate, continues to be put into sealing and standing 1 day in the insulating box that temperature is 30 DEG C, mixed liquor is obtained, by mixed liquor high temperature
Sterilization tank obtains sterilizing mixed liquor with 120 DEG C of temperature sterilizing 10min；It counts in parts by weight, 1 part is added in into three-necked flask
OP-10,0.5 part of SE-10,1 part of sodium bicarbonate and 100 parts of water, stirring and dissolving 10min obtain mixed solution, then to three-necked flask
10 parts of vinyl acetates of middle addition, 8 parts of butyl acrylates, 12 parts of hydroxy-ethyl acrylates, 9 parts of acrylic acid, are stirred 10min and obtain
To prefabricated solution；Three-necked flask is moved into water-bath, 70 DEG C is heated to, is added dropwise with constant pressure funnel into three-necked flask
The mass fraction of prefabricated solution quality 10% is 5% ammonium persulfate solution, and control drop rate makes ammonium persulfate solution be dripped in 25min
It adds complete, is warming up to 85 DEG C after insulated and stirred reaction 2h, continues to be stirred to react 20min, it is water-fast height that discharging, which obtains reaction solution,
Sticky paper-plastic lamination adhesive.
Example 2
It is 1 in mass ratio:5:1 will be put into after orthosilicic acid and the mixing of water and Silane coupling agent KH550 in reaction kettle, sealing reaction
155 DEG C are heated in kettle, starts blender, is filtered after being stirred to react 1h with the rotating speed of 250r/min, isolated filter residue；
It is 4 in mass ratio by filter residue and vinylbenzyltrimethyl ammonium chloride and water:1:After 38 mixing, mixed liquor is obtained, will be mixed
Liquid is fitted into reaction kettle, then a concentration of 50mmol/L hydrogen peroxide of mixed liquor quality 40% and mixed liquor matter are added in into reaction kettle
The solution of ferrous chloride of a concentration of 0.1mol/L of amount 5% and the benzoyl peroxide of mixed liquor quality 1%, sealing reaction kettle add
Heat is warming up to 110 DEG C, is separated by filtration to obtain filter cake after being stirred to react 1h, as cation modified nano silicon dioxide；By weight
Number meter weighs 45 parts of cation modified nano silicon dioxides, 18 parts of wood tar, 8 parts of starch and 18 parts a concentration of 107cfu/mL
Ruminococcus albus bacteria suspension be fitted into fermentation tank, sealing tank mouth is sealed by fermentation 8 days at 28 DEG C, and filtering after fermentation divides
From fermentation filter residue is obtained, nano silicon dioxide is modified up to modified cation after sterilizing；Tea polyphenols and biogas slurry are pressed and wait mass ratioes
Blending is placed on sealing and standing 6 days in the insulating box that temperature is 35 DEG C, filtrate is obtained by filtration, then is 1 in mass ratio:3 by xanthans
It is blended with filtrate, continues to be put into sealing and standing 1 day in the insulating box that temperature is 35 DEG C, mixed liquor is obtained, by mixed liquor high temperature
Sterilization tank obtains sterilizing mixed liquor with 120 DEG C of temperature sterilizing 13min；It counts in parts by weight, 1 part is added in into three-necked flask
OP-10,0.7 part of SE-10,2 parts of sodium bicarbonates and 130 parts of water, stirring and dissolving 13min obtain mixed solution, then to three-necked flask
13 parts of vinyl acetates of middle addition, 9 parts of butyl acrylates, 14 parts of hydroxy-ethyl acrylates, 11 parts of acrylic acid, are stirred 13min
Obtain prefabricated solution；Three-necked flask is moved into water-bath, 75 DEG C is heated to, is dripped with constant pressure funnel into three-necked flask
The mass fraction for adding prefabricated solution quality 10% is 5% ammonium persulfate solution, and control drop rate makes ammonium persulfate solution in 28min
It is added dropwise, 90 DEG C is warming up to after insulated and stirred reaction 3h, continue to be stirred to react 25min, it is as water-fast that discharging obtains reaction solution
High viscosity paper-plastic lamination adhesive.
Example 3
It is 1 in mass ratio:5:1 will be put into after orthosilicic acid and the mixing of water and Silane coupling agent KH550 in reaction kettle, sealing reaction
160 DEG C are heated in kettle, starts blender, is filtered after being stirred to react 2h with the rotating speed of 300r/min, isolated filter residue；
It is 4 in mass ratio by filter residue and vinylbenzyltrimethyl ammonium chloride and water:1:After 38 mixing, mixed liquor is obtained, will be mixed
Liquid is fitted into reaction kettle, then a concentration of 50mmol/L hydrogen peroxide of mixed liquor quality 40% and mixed liquor matter are added in into reaction kettle
The solution of ferrous chloride of a concentration of 0.1mol/L of amount 5% and the benzoyl peroxide of mixed liquor quality 1%, sealing reaction kettle add
Heat is warming up to 120 DEG C, is separated by filtration to obtain filter cake after being stirred to react 2h, as cation modified nano silicon dioxide；By weight
Number meter weighs 50 parts of cation modified nano silicon dioxides, 20 parts of wood tar, 10 parts of starch and 20 parts a concentration of 107cfu/
The Ruminococcus albus bacteria suspension of mL is fitted into fermentation tank, and sealing tank mouth is sealed by fermentation 9 days at 30 DEG C, is filtered after fermentation
Isolated fermentation filter residue modifies nano silicon dioxide after sterilizing up to modified cation；By tea polyphenols and biogas slurry by etc. quality
Than blending, sealing and standing 7 days in the insulating box that temperature is 40 DEG C are placed on, filtrate is obtained by filtration, then be 1 in mass ratio:3 by xanthan
Glue and filtrate blending continue to be put into sealing and standing 2 days in the insulating box that temperature is 40 DEG C, obtain mixed liquor, by mixed liquor height
Warm sterilization tank obtains sterilizing mixed liquor with 120 DEG C of temperature sterilizing 15min；It counts in parts by weight, 2 is added in into three-necked flask
Part OP-10,0.8 part of SE-10,3 parts of sodium bicarbonates and 150 parts of water, stirring and dissolving 15min obtain mixed solution, then to three mouthfuls
15 parts of vinyl acetates, 10 parts of butyl acrylates, 15 parts of hydroxy-ethyl acrylates, 12 parts of acrylic acid are added in flask, are stirred
15min obtains prefabricated solution；Three-necked flask is moved into water-bath, is heated to 80 DEG C, is burnt with constant pressure funnel to three mouthfuls
The mass fraction that prefabricated solution quality 10% is added dropwise in bottle is 5% ammonium persulfate solution, and control drop rate makes ammonium persulfate solution exist
It is added dropwise in 30min, 95 DEG C is warming up to after insulated and stirred reaction 4h, continue to be stirred to react 30min, discharging obtains reaction solution i.e.
For water-fast high viscosity paper-plastic lamination adhesive.
Reference examples
Using the paper-plastic lamination adhesive that Guangzhou company produces as reference examples
Performance detection is carried out to the Laminating adhesive in Laminating adhesive produced by the present invention and reference examples, testing result is as shown in table 1：
Table 1：
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Paper viscosity（mPa· s） | 55 | 57 | 59 | 46 |
| Tack（min） | 8.5 | 8.9 | 9.6 | 7.8 |
| Hold viscosity（h） | 65 | 68 | 70 | 50 |
| 180 ° of peel strengths （N·25mm-1） | 6.5 | 7.2 | 7.4 | 5.0 |
| Heat drying stability | 30h is not blistering at 60 DEG C, not delamination | 35h is not blistering at 60 DEG C, not delamination | 40h is not blistering at 60 DEG C, not delamination | It is not blistering for 24 hours at 60 DEG C, it does not take off Layer |
| Water-resistance | It is removed after 110 DEG C of hot-water soak 10min Intensity is unchanged | It is removed after 110 DEG C of hot-water soak 15min Intensity is unchanged | It is removed after 110 DEG C of hot-water soak 18min Intensity is unchanged | After 110 DEG C of hot-water soak 5min Peel strength is unchanged |
Paper-plastic lamination adhesive produced by the present invention has splendid water resistance, adhesion strength it can be seen from detection data in upper table
Height, and stable mechanical performance, have broad application prospects.
Claims (6)
1. a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive, it is characterised in that specifically preparation process is：
（1）It is put into reaction kettle after orthosilicic acid and water and Silane coupling agent KH550 are mixed, seals heat temperature raising in reaction kettle
It to 150~160 DEG C, is filtered after being stirred to react 1~2h, isolated filter residue；
（2）After above-mentioned filter residue and vinylbenzyltrimethyl ammonium chloride and water are mixed, mixed liquor is obtained, mixed liquor is packed into
In reaction kettle, then hydrogen peroxide and solution of ferrous chloride and benzoyl peroxide are added in into reaction kettle, sealing reaction kettle heating
100~120 DEG C are warming up to, is separated by filtration to obtain filter cake after being stirred to react 1~2h, as cation modified nano silicon dioxide；
（3）Count in parts by weight, weigh 40~50 parts of above-mentioned cation modified nano silicon dioxides, 15~20 parts of wood tar, 5~
10 parts of starch and 15~20 parts a concentration of 107The Ruminococcus albus bacteria suspension of cfu/mL is fitted into fermentation tank, is sealed by fermentation, hair
It is separated by filtration to obtain fermentation filter residue after ferment, nano silicon dioxide is modified up to modified cation after sterilizing；
（4）By tea polyphenols and biogas slurry by mass ratioes blending is waited, sealing and standing 5~7 days in insulating box are placed on, filtrate is obtained by filtration,
Xanthans and filtrate are blended again, continues to be put into sealing and standing 1~2 day in insulating box, obtains mixed liquor, mixed liquor high temperature is gone out
Bacterium obtains sterilizing mixed liquor；
（5）It counts in parts by weight, 1~2 part of OP-10,0.5~0.8 part of SE-10,1~3 part of bicarbonate is added in into three-necked flask
Sodium and 100~150 parts of water, 10~15min of stirring and dissolving obtains mixed solution, then 10~15 parts of acetic acid are added in into three-necked flask
Vinyl acetate, 8~10 parts of butyl acrylates, 12~15 parts of hydroxy-ethyl acrylates, 9~12 parts of acrylic acid, are stirred 10~15min
Obtain prefabricated solution；
（6）Above-mentioned three-necked flask is moved into water-bath, is heated to 70~80 DEG C, with constant pressure funnel to three-necked flask
Middle dropwise addition ammonium persulfate solution, control drop rate make ammonium persulfate solution be added dropwise in 25~30min, and insulated and stirred is anti-
85~95 DEG C are warming up to after answering 2~4h, continues to be stirred to react 20~30min, it is water-fast high viscosity paper that discharging, which obtains reaction solution,
Mould Laminating adhesive.
2. a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive according to claim 1, it is characterised in that：Step
（1）Described in orthosilicic acid and water and Silane coupling agent KH550 be 1 in mass ratio:5:1.
3. a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive according to claim 1, it is characterised in that：Step
（2）Described in filter residue and the mass ratio of vinylbenzyltrimethyl ammonium chloride and water be 4:1:38, the addition of hydrogen peroxide
It is the 40% of mixed liquor quality, a concentration of 50mmol/L of hydrogen peroxide, the addition of solution of ferrous chloride is mixed liquor quality
5%, a concentration of 0.1mol/L of solution of ferrous chloride, the addition of benzoyl peroxide are the 1% of mixed liquor quality.
4. a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive according to claim 1, it is characterised in that：Step
（3）Described in sealing and fermenting temperature for 25~30 DEG C, the time of sealing and fermenting is 7~9 days.
5. a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive according to claim 1, it is characterised in that：Step
（4）Described in insulating box temperature for 30~40 DEG C, the mass ratio of xanthans and filtrate is 1:3, the temperature of high-temperature sterilization is
120 DEG C, the time of high-temperature sterilization is 10~15min.
6. a kind of preparation method of water-fast high viscosity paper-plastic lamination adhesive according to claim 1, it is characterised in that：Step
（6）Described in the dripping quantity of ammonium persulfate solution be the 10% of prefabricated solution quality, the mass fraction of ammonium persulfate solution is 5%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113980611A (en) * | 2021-10-13 | 2022-01-28 | 柳宙新材料(宁波)有限公司 | Outdoor high-weatherability acrylic pressure-sensitive adhesive for reflective film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266263A (en) * | 2018-08-31 | 2019-01-25 | 王成 | A kind of preparation method of high viscosity Laminating adhesive |
| CN113980611A (en) * | 2021-10-13 | 2022-01-28 | 柳宙新材料(宁波)有限公司 | Outdoor high-weatherability acrylic pressure-sensitive adhesive for reflective film |
| CN113980611B (en) * | 2021-10-13 | 2024-01-23 | 柳宙新材料(宁波)有限公司 | High weather resistance acrylic pressure-sensitive adhesive outside reflective film user |
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