CN109054658A - A kind of preparation method of the high viscous adhesive of environmental protection - Google Patents
A kind of preparation method of the high viscous adhesive of environmental protection Download PDFInfo
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- CN109054658A CN109054658A CN201810944295.6A CN201810944295A CN109054658A CN 109054658 A CN109054658 A CN 109054658A CN 201810944295 A CN201810944295 A CN 201810944295A CN 109054658 A CN109054658 A CN 109054658A
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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
- C09J1/00—Adhesives based on inorganic constituents
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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
Abstract
The invention discloses a kind of preparation methods of the high viscous adhesive of environmental protection, comprising the following steps: preparation premix A, prepares tackifying assistant, passes through the high viscous adhesive of the environmental protection for being stirred to react and being invented with natural gum juice, diatomite in powder and auxiliary agent again.Wallpaper adhesive of the present invention is using graphene as basis material, by graphene through superoxidized modified, improve the activity of graphene, and then enhance the active force between raw material, simultaneously by rare earth oxide, mica powder and stratiform hypophosphites pass through ultrasonic disperse, it is inserted into modified graphene, the architecture of formation is stablized, then adhesion is enhanced, the features such as weatherability, the hydroxypropul starch of addition has thickening power, the tackifying assistant of addition effectively increases the caking property and film forming of adhesive, convenient for adhesive construction, diatomite in powder can further promote to mix between raw material, the stabilization of enhancing system.
Description
Technical field
The present invention relates to wallpaper adhesive preparation technical fields, and in particular to a kind of preparation side of the high viscous adhesive of environmental protection
Method.
Background technique
Wallpaper is bonded adhesive, which is divided into water base class and powdery type, water base class be divided into again Water-soluble adhesive with
Emulsion-type adhesive, powdered wallpaper adhesive all have the characteristics that instant, tasteless, nontoxic, not mould, and Water-soluble adhesive has can
Soluble starch glue, carboxymethyl cellulose gum, denaturation soluble starch glue, polyvinyl alcohol etc., emulsion-type adhesive has poly-vinegar acid second
Alkene lotion, acrylic acid ester emulsion, epoxy resin latex etc., it is powdered to have starch and its derivative, cellulose and its derivates, tree
Lipid, wallpaper adhesive have biggish polarity, can be preferably bonded, good fluidity, have heat resistance, have water resistance,
Poly- alkali resistance.
Existing Chinese patent literature (notification number: CN106753224B) discloses a kind of environment protection type wallpaper adhesive and its system
Preparation Method, including A agent and B agent；A agent is formed by the Raw material processing of following parts by weight: modified 60-80 parts of defatted soy flour cream, water-soluble
Property 6-8 parts of glucan, 4-6 parts of levelling agent, 2-3 parts of organobentonite, 1-3 parts of auxiliary agent, auxiliary agent be fireproof powder, nanometer anion powder
With at least two mixture in antistatic agent；B agent is formed by the Raw material processing of following parts by weight: 8-15 parts of bee glue powder, being resisted
1-3 parts of oxidant, 30-40 parts of matrix, 1-2 parts of emulsifier, 40-60 parts of volume fraction 75-85% alcohol solvent, which exists
Peel strength is good under room temperature, but temperature improves, and peel strength can be deteriorated, therefore need to prepare a kind of adhesive that stability is good.
Summary of the invention
It in view of the drawbacks of the prior art, should the object of the present invention is to provide a kind of preparation method of the high viscous adhesive of environmental protection
Adhesive is environmentally protective, and adhesive strength is good, while performance is stablized.
The present invention solves technical problem and adopts the following technical scheme that
The present invention provides a kind of preparation methods of the high viscous adhesive of environmental protection, comprising the following steps:
Step 1 weighs 44-48 parts of modified graphene and is added in reaction kettle according to parts by weight, adjusts temperature and is
55-65 DEG C, 15-25min is reacted, 62-68 parts of mass fraction 40-50% hydrochloric acid solutions are then added thereto, are configured to be modified
12-16 parts of hydroxypropul starch, 16-22 parts of ethanol solution is then added in graphene dispersing solution thereto again, stirs 15-
25min then adds 8-14 parts of stratiform hypophosphites, carries out ultrasonic disperse 15-25min, obtains premix A；
The preparation method of the modified graphene is that graphene is added in magnetic stirring apparatus, then adds nitration mixture,
Whipping temp is 65-75 DEG C, stirs 15-25min, then washes, filters again, dry to get modified graphene；
Casein is added in the deionized water of 6-8 times of its weight, stirs evenly by step 2, ultrasonic disperse 3-5min,
Adding and accounting for mixed liquor quality 2-4% organic alcohol amine compound adjusting pH value is 7-8, is stirred to react 30-45min, obtains casein
Liquid；Casein liquid and epoxy resin are mixed according to weight ratio 10:1 again, 20-25min is mixed under the conditions of 20-25 DEG C and obtains
The butyl glycol ether and hydroxyethyl methacrylate for accounting for the composition of 1:2 in mass ratio of mixed liquor weight 12-14% is added in mixed liquor
Mixed solvent is placed in the four-hole bottle equipped with blender, constant pressure funnel, condenser pipe and nitrogen conduit, using the side of polymerisation in solution
Method is slowly stirred and is warming up to 70-80 DEG C, obtains polymer solution, add account for polymer solution 8-10% be in mass ratio
The zinc acetate of 1:2 composition and the mixed liquor of acid anhydrides, are to slowly warm up to acid anhydrides and when zinc acetate is completely dissolved under nitrogen protection, side
Stirring side is warming up to 250-280 DEG C, and insulation reaction 2-3h is cooled to 200-220 DEG C, obtains mixture B；
Step 3, in mass ratio 2:3:4:1:2 are sub- by polyester resin, isocyanates, peach gum, mixture B and trimethyl six
Methanediamine is added in reaction kettle, and keeping temperature is 180-200 DEG C, is stirred to react 1-2h, is cooled to room temperature to obtain to viscosify and help
Agent；
Step 4, according to parts by weight, by the increasing of A, 15-20 parts of step 3 of the premix preparation in 50-60 parts of step 1
Viscous auxiliary agent, 5-10 parts of natural gum juice, 8-10 parts of diatomites in powder, are added in blender, first carry out high-speed stirring with 135-145r/min
35-45min is mixed, 3-5 parts of auxiliary agents is then added, is stirred at low speed with 75-85r/min, stirs 45min to get the present invention
The high viscous adhesive of environmental protection.
Preferably, the mixture that the nitration mixture is the concentrated sulfuric acid, concentrated nitric acid is formed according to weight ratio 2:1.
Preferably, the hydroxypropul starch preparation method is that starch is added in reaction flask, and sodium sulphate, hydrogen is then added
Sodium oxide molybdena is filled with nitrogen, then adds propylene oxide, stirs 15-25min, and then adding mass fraction is that 50-60% is dilute
Sulfuric acid until solution is neutrality, then is centrifuged, washes, dries to get hydroxypropul starch.
Preferably, the preparation method of layered hypophosphites is by aluminium chloride, sodium hypophosphite, polyoxyethylene-polyoxy third
Alkene copolymer is placed in autoclave, and dehydrated alcohol is added, and rare earth oxide, mica powder is then added in stirring thereto again, into
Row ultrasonic disperse 15-25min, is subsequently placed in baking oven and handles 3.5h, then filter, washing, then is placed in drying, grinding in baking oven and is
For stratiform hypophosphites, stratiform hypophosphites is finally subjected to sided corona treatment 5-9min.
Preferably, the rare earth oxide is cerium oxide.
Preferably, the sided corona treatment power is 5KW, and treatment temperature is 45 DEG C.
Preferably, the mixture that the natural gum juice is pin tree sap, Bajiao Banana Juice is formed according to weight ratio 4:1.
Preferably, the diatomite in powder is the high-quality diatomite ore of silica containing 90%, and by calcining, calcination temperature is
850-950 DEG C, 25min is calcined, then crushes to be sent into sorting machine and sort.
Preferably, the auxiliary agent is sodium tripolyphosphate, lignin is mixed according to weight ratio 5:2.
Compared with prior art, the present invention have it is following the utility model has the advantages that
(1) wallpaper adhesive of the present invention is using graphene as basis material, and seldom occurs in existing literature graphene-based
As wallpaper adhesive technology field application, by graphene through superoxidized modified, improve the activity of graphene, so enhance with it is former
Active force between material, and stratiform hypophosphites has laminated structure, rare earth oxide, mica powder and stratiform hypophosphites pass through
Rare earth oxide, mica powder are attached in its laminated structure by ultrasonic disperse, then by sided corona treatment, make material adhesion more
Good, then stratiform hypophosphites is inserted into modified graphene, the architecture of formation is stablized, and then enhances adhesion, weather-proof
Property the features such as, the hydroxypropul starch of addition has thickening power, constructs convenient for adhesive, and diatomite in powder can further promote original
It is mixed between material, enhances the stabilization of system.
(2) simultaneously because the present invention is by containing the very high ring of reactivity under alkaline environment in epoxy molecule
Oxygroup, which reacts with the hydrophilic radicals such as amino, carboxyl and hydroxyl in casein, to improve tackifying assistant
Water resistance and wet-rub resistance block the intermediate polarity group of casein strand to be formed by adding polyester resin, isocyanates, peach gum
Hydrogen bond, to improve the adhesive property of tackifying assistant, polyester resin, isocyanates, peach gum and extract solution from aloe addition are not only risen
To the addition for reducing epoxy resin and casein, cost is reduced, the stringiness for reducing entire material adhesive is also acted as, protects simultaneously
It is best to demonstrate,prove performance of the material in bonding；Acid anhydrides and zinc acetate is added, in addition to improving viscosity, the drying time of material is also made to contract
Short and water resistance improves；Interaction between casein and epoxy molecule, the product for improving modified Casein resin stretch
Performance, elongation at break increase, and add trimethylhexamethylenediamine, play thickening solidification to epoxy resin, improve
Toughness, viscosity and the corrosion resistance of adhesive.
(3) it obtains from embodiment 3 and comparative example 1-3, peel strength, measured at 40 DEG C and measures at room temperature, this hair
It is bright very big with the influence change of comparative example 3, it is measured after 1 week at 40 DEG C, the present invention improves 0.37N/mm, room relative to comparative example 3
Temperature measures after lower 1 week, improves 0.1N/mm, it is known that, peel strength of the present invention is with significant advantage at 40 DEG C, and in sweltering heat
Regional high temperature season, room temperature can reach 36-42 DEG C, therefore the present invention is more suitable for this area's use, and stratiform hypophosphites is to removing
Intensity, bonding strength, which have, to be significantly affected, and is added stratiform hypophosphites, is measured after 1 week at 40 DEG C, peel strength improves
0.33N/mm, improvement rate 28.44%.
Specific embodiment
Combined with specific embodiments below, technical scheme in the embodiment of the invention is clearly and completely described, shows
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1.
A kind of preparation method of the high viscous adhesive of the environmental protection of the present embodiment, comprising the following steps:
Step 1 weighs 44 parts of modified graphene and is added in reaction kettle according to parts by weight, and adjusting temperature is 55
DEG C, 15min is reacted, 62 parts of 40% hydrochloric acid solutions of mass fraction are then added thereto, are configured to modified graphene dispersion liquid, with
12 parts of hydroxypropul starch, 16 parts of ethanol solution is added thereto again afterwards, stirs 15min, then adds 8 parts of stratiforms time phosphorus
Hydrochlorate carries out ultrasonic disperse 15min, obtains premix A；
Casein is added in the deionized water of 6 times of its weight, stirs evenly by step 2, ultrasonic disperse 3min, then plus
Entering to account for 2% organic alcohol amine compound of mixed liquor quality to adjust pH value is 7-8, is stirred to react 30min, obtains casein liquid；Again by junket
Plain liquid and epoxy resin are mixed according to weight ratio 10:1, and 20min is mixed at 20 °C and obtains mixed liquor, addition accounts for mixed
The butyl glycol ether and hydroxyethyl methacrylate mixed solvent for closing the composition of 1:2 in mass ratio of liquid weight 12%, are placed in and are equipped with
Blender, constant pressure funnel, condenser pipe and nitrogen conduit four-hole bottle in, using the method for polymerisation in solution, be slowly stirred and be warming up to
70 DEG C, polymer solution is obtained, adding account for polymer solution 8% is in mass ratio the zinc acetate and acid anhydrides of 1:2 composition
Mixed liquor, is to slowly warm up to acid anhydrides under nitrogen protection and when zinc acetate is completely dissolved, warming while stirring is to 250 DEG C, heat preservation
2h is reacted, 200 DEG C is cooled to, obtains mixture B；
Step 3, in mass ratio 2:3:4:1:2 are sub- by polyester resin, isocyanates, peach gum, mixture B and trimethyl six
Methanediamine is added in reaction kettle, and keeping temperature is 180 DEG C, is stirred to react 1h, is cooled to room temperature to obtain tackifying assistant；
Step 4, according to parts by weight, by the tackifying assistant of premix A, the preparation of 15 parts of step 3 in 50 parts of step 1,
5 parts of natural gum juice, 8 parts of diatomites in powder are added in blender, first carry out high-speed stirred 35min with 135r/min, then add
3 parts of auxiliary agents, are stirred at low speed with 75r/min, stir 45min to get the high viscous adhesive of environmental protection of the invention.
The preparation method of modified graphene in the present embodiment is that graphene is added in magnetic stirring apparatus, is then added again
Enter nitration mixture, whipping temp is 65 DEG C, stirs 15min, then washes, filters again, dry to get modified graphene.
Nitration mixture in the present embodiment is the mixture that the concentrated sulfuric acid, concentrated nitric acid are formed according to weight ratio 2:1.
Hydroxypropul starch preparation method in the present embodiment is that starch is added in reaction flask, be then added sodium sulphate,
Sodium hydroxide is filled with nitrogen, then adds propylene oxide, stirs 15min, and then adding mass fraction is 50% dilute sulphur
Acid until solution is neutrality, then is centrifuged, washes, dries to get hydroxypropul starch.
The preparation method of stratiform hypophosphites in the present embodiment is by aluminium chloride, sodium hypophosphite, polyoxyethylene-polyoxy third
Alkene copolymer is placed in autoclave, and dehydrated alcohol is added, and rare earth oxide, mica powder is then added in stirring thereto again, into
Row ultrasonic disperse 15min, is subsequently placed in baking oven and handles 3.5h, then filter, washing, then is placed in drying, grinding in baking oven and is
Stratiform hypophosphites is finally carried out sided corona treatment 5min by stratiform hypophosphites.
Rare earth oxide in the present embodiment is cerium oxide.
Sided corona treatment power in the present embodiment is 5KW, and treatment temperature is 45 DEG C.
Natural gum juice in the present embodiment is the mixture that pin tree sap, Bajiao Banana Juice are formed according to weight ratio 4:1.
Diatomite in powder in the present embodiment is the high-quality diatomite ore of silica containing 90%, by calcining, calcination temperature
It is 850-950 DEG C, calcines 25min, then crushes to be sent into sorting machine and sort.
Auxiliary agent in the present embodiment is sodium tripolyphosphate, lignin is mixed according to weight ratio 5:2.
Embodiment 2.
A kind of preparation method of the high viscous adhesive of the environmental protection of the present embodiment, comprising the following steps:
Step 1 weighs 48 parts of modified graphene and is added in reaction kettle according to parts by weight, and adjusting temperature is 65
DEG C, 25min is reacted, 68 parts of 50% hydrochloric acid solutions of mass fraction are then added thereto, are configured to modified graphene dispersion liquid, with
16 parts of hydroxypropul starch, 22 parts of ethanol solution is added thereto again afterwards, stirs 25min, then adds 14 parts of stratiforms time
Phosphate carries out ultrasonic disperse 25min, obtains premix A；
Casein is added in the deionized water of 8 times of its weight, stirs evenly by step 2, ultrasonic disperse 5min, then plus
Entering to account for 4% organic alcohol amine compound of mixed liquor quality to adjust pH value is 7-8, is stirred to react 45min, obtains casein liquid；Again by junket
Plain liquid and epoxy resin are mixed according to weight ratio 10:1, and 25min is mixed under the conditions of 25 DEG C and obtains mixed liquor, addition accounts for mixed
The butyl glycol ether and hydroxyethyl methacrylate mixed solvent for closing the composition of 1:2 in mass ratio of liquid weight 14%, are placed in and are equipped with
Blender, constant pressure funnel, condenser pipe and nitrogen conduit four-hole bottle in, using the method for polymerisation in solution, be slowly stirred and be warming up to
80 DEG C, polymer solution is obtained, adding account for polymer solution 10% is in mass ratio the zinc acetate and acid anhydrides of 1:2 composition
Mixed liquor, is to slowly warm up to acid anhydrides under nitrogen protection and when zinc acetate is completely dissolved, warming while stirring is to 280 DEG C, heat preservation
3h is reacted, 220 DEG C is cooled to, obtains mixture B；
Step 3, in mass ratio 2:3:4:1:2 are sub- by polyester resin, isocyanates, peach gum, mixture B and trimethyl six
Methanediamine is added in reaction kettle, and keeping temperature is 200 DEG C, is stirred to react 2h, is cooled to room temperature to obtain tackifying assistant；
Step 4, according to parts by weight, by the tackifying assistant of premix A, the preparation of 20 parts of step 3 in 60 parts of step 1,
10 parts of natural gum juice, 10 parts of diatomites in powder are added in blender, first carry out high-speed stirred 45min with 145r/min, then add again
Enter 5 parts of auxiliary agents, stirred at low speed with 85r/min, stirs 45min to get the high viscous adhesive of environmental protection of the invention.
The preparation method of modified graphene in the present embodiment is that graphene is added in magnetic stirring apparatus, is then added again
Enter nitration mixture, whipping temp is 75 DEG C, stirs 25min, then washes, filters again, dry to get modified graphene.
Nitration mixture in the present embodiment is the mixture that the concentrated sulfuric acid, concentrated nitric acid are formed according to weight ratio 2:1.
Hydroxypropul starch preparation method in the present embodiment is that starch is added in reaction flask, be then added sodium sulphate,
Sodium hydroxide is filled with nitrogen, then adds propylene oxide, stirs 25min, and then adding mass fraction is 60% dilute sulphur
Acid until solution is neutrality, then is centrifuged, washes, dries to get hydroxypropul starch.
The preparation method of stratiform hypophosphites in the present embodiment is by aluminium chloride, sodium hypophosphite, polyoxyethylene-polyoxy third
Alkene copolymer is placed in autoclave, and dehydrated alcohol is added, and rare earth oxide, mica powder is then added in stirring thereto again, into
Row ultrasonic disperse 25min, is subsequently placed in baking oven and handles 3.5h, then filter, washing, then is placed in drying, grinding in baking oven and is
Stratiform hypophosphites is finally carried out sided corona treatment 9min by stratiform hypophosphites.
Rare earth oxide in the present embodiment is cerium oxide.
Sided corona treatment power in the present embodiment is 5KW, and treatment temperature is 45 DEG C.
Natural gum juice in the present embodiment is the mixture that pin tree sap, Bajiao Banana Juice are formed according to weight ratio 4:1.
Diatomite in powder in the present embodiment is the high-quality diatomite ore of silica containing 90%, by calcining, calcination temperature
It is 850-950 DEG C, calcines 25min, then crushes to be sent into sorting machine and sort.
Auxiliary agent in the present embodiment is sodium tripolyphosphate, lignin is mixed according to weight ratio 5:2.
Embodiment 3.
A kind of preparation method of the high viscous adhesive of the environmental protection of the present embodiment, comprising the following steps:
Step 1 weighs 46 parts of modified graphene and is added in reaction kettle according to parts by weight, and adjusting temperature is 60
DEG C, 20min is reacted, 65 parts of 45% hydrochloric acid solutions of mass fraction are then added thereto, are configured to modified graphene dispersion liquid, with
14 parts of hydroxypropul starch, 19 parts of ethanol solution is added thereto again afterwards, stirs 20min, then adds 11 parts of stratiforms time
Phosphate carries out ultrasonic disperse 20min, obtains premix A；
Casein is added in the deionized water of 7 times of its weight, stirs evenly by step 2, ultrasonic disperse 4min, then plus
Entering to account for 3% organic alcohol amine compound of mixed liquor quality to adjust pH value is 7-8, is stirred to react 37min, obtains casein liquid；Again by junket
Plain liquid and epoxy resin are mixed according to weight ratio 10:1, and 22min is mixed under the conditions of 22 DEG C and obtains mixed liquor, addition accounts for mixed
The butyl glycol ether and hydroxyethyl methacrylate mixed solvent for closing the composition of 1:2 in mass ratio of liquid weight 13%, are placed in and are equipped with
Blender, constant pressure funnel, condenser pipe and nitrogen conduit four-hole bottle in, using the method for polymerisation in solution, be slowly stirred and be warming up to
75 DEG C, polymer solution is obtained, adding account for polymer solution 9% is in mass ratio the zinc acetate and acid anhydrides of 1:2 composition
Mixed liquor, is to slowly warm up to acid anhydrides under nitrogen protection and when zinc acetate is completely dissolved, warming while stirring is to 265 DEG C, heat preservation
2.5h is reacted, 210 DEG C is cooled to, obtains mixture B；
Step 3, in mass ratio 2:3:4:1:2 are sub- by polyester resin, isocyanates, peach gum, mixture B and trimethyl six
Methanediamine is added in reaction kettle, and keeping temperature is 190 DEG C, is stirred to react 1.5h, is cooled to room temperature to obtain tackifying assistant；
Step 4, according to parts by weight, by the tackifying assistant of premix A, the preparation of 18 parts of step 3 in 55 parts of step 1,
8 parts of natural gum juice, 9 parts of diatomites in powder are added in blender, first carry out high-speed stirred 40min with 140r/min, then add
4 parts of auxiliary agents, are stirred at low speed with 80r/min, stir 45min to get the high viscous adhesive of environmental protection of the invention.
The preparation method of modified graphene in the present embodiment is that graphene is added in magnetic stirring apparatus, is then added again
Enter nitration mixture, whipping temp is 70 DEG C, stirs 20min, then washes, filters again, dry to get modified graphene.
Nitration mixture in the present embodiment is the mixture that the concentrated sulfuric acid, concentrated nitric acid are formed according to weight ratio 2:1.
Hydroxypropul starch preparation method in the present embodiment is that starch is added in reaction flask, be then added sodium sulphate,
Sodium hydroxide is filled with nitrogen, then adds propylene oxide, stirs 20min, and then adding mass fraction is 55% dilute sulphur
Acid until solution is neutrality, then is centrifuged, washes, dries to get hydroxypropul starch.
The preparation method of stratiform hypophosphites in the present embodiment is by aluminium chloride, sodium hypophosphite, polyoxyethylene-polyoxy third
Alkene copolymer is placed in autoclave, and dehydrated alcohol is added, and rare earth oxide, mica powder is then added in stirring thereto again, into
Row ultrasonic disperse 20min, is subsequently placed in baking oven and handles 3.5h, then filter, washing, then is placed in drying, grinding in baking oven and is
Stratiform hypophosphites is finally carried out sided corona treatment 7min by stratiform hypophosphites.
Rare earth oxide in the present embodiment is cerium oxide.
Sided corona treatment power in the present embodiment is 5KW, and treatment temperature is 45 DEG C.
Natural gum juice in the present embodiment is the mixture that pin tree sap, Bajiao Banana Juice are formed according to weight ratio 4:1.
Diatomite in powder in the present embodiment is the high-quality diatomite ore of silica containing 90%, by calcining, calcination temperature
It is 900 DEG C, calcines 25min, then crushes to be sent into sorting machine and sort.
Auxiliary agent in the present embodiment is sodium tripolyphosphate, lignin is mixed according to weight ratio 5:2.
Comparative example 1.
It is essentially identical with the material and preparation process of embodiment 3, it has only the difference is that being not added with stratiform hypophosphites.
Comparative example 2.
It is essentially identical with the material and preparation process of embodiment 3, it has only the difference is that being not added with diatomite in powder.
Comparative example 3.
A kind of environment protection type wallpaper adhesive and its system are disclosed using Chinese patent literature (notification number: CN106753224B)
The raw material and method of embodiment 3 in Preparation Method.
The present invention at room temperature, temperature be 40 DEG C at the performance of adhesive is probed into
Embodiment 3 and comparative example 1-3 the performance test results are as follows
Obtained from embodiment 3 and comparative example 1-3, peel strength, at 40 DEG C measurement with measure at room temperature, the present invention and
The influence change of comparative example 3 is very big, measures after 1 week at 40 DEG C, the present invention improves 0.37N/mm, at room temperature relative to comparative example 3
It is measured after 1 week, improves 0.1N/mm, it is known that, peel strength of the present invention has significant advantage at 40 DEG C, and in hot area
High temperature season, room temperature can reach 36-42 DEG C, therefore the present invention is more suitable for this area's use, stratiform hypophosphites to peel strength,
Bonding strength, which has, to be significantly affected, and is added stratiform hypophosphites, is measured after 1 week at 40 DEG C, and peel strength improves 0.33N/mm,
Improvement rate is 28.44%.
Had a significant impact based on the pleasantly surprised discovery stratiform hypophosphites of the studies above present invention to adhesive property tool, therefore this
Invention further studies stratiform hypophosphites preparation process to probe into and influence adhesive property.
Performance study is as follows
It is obtained from experimental example 1-3, using conventional stratiform hypophosphites preparation process, with phosphate prepared by the present invention
Bonding strength, peel strength differ greatly, in addition, rare earth oxide is greater than mica powder to adhesive bonding strength, peel strength
Influence to adhesive bonding strength, peel strength.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of preparation method of the high viscous adhesive of environmental protection, which comprises the following steps:
Step 1 weighs 44-48 parts of modified graphene and is added in reaction kettle according to parts by weight, and adjusting temperature is 55-65
DEG C, 15-25min is reacted, 62-68 parts of mass fraction 40-50% hydrochloric acid solutions are then added thereto, are configured to modified graphene
12-16 parts of hydroxypropul starch, 16-22 parts of ethanol solution is then added in dispersion liquid thereto again, stirs 15-25min, with
After add 8-14 parts of stratiform hypophosphites, carry out ultrasonic disperse 15-25min, obtain premix A；
The preparation method of the modified graphene is that graphene is added in magnetic stirring apparatus, then adds nitration mixture, is stirred
Temperature is 65-75 DEG C, stirs 15-25min, then washes, filters again, dry to get modified graphene；
Casein is added in the deionized water of 6-8 times of its weight, stirs evenly by step 2, ultrasonic disperse 3-5min, then plus
Entering to account for mixed liquor quality 2-4% organic alcohol amine compound to adjust pH value is 7-8, is stirred to react 30-45min, obtains casein liquid；Again
Casein liquid and epoxy resin are mixed according to weight ratio 10:1,20-25min is mixed under the conditions of 20-25 DEG C and is mixed
The butyl glycol ether for accounting for the composition of 1:2 in mass ratio of mixed liquor weight 12-14% and hydroxyethyl methacrylate mixing is added in liquid
Solvent is placed in the four-hole bottle equipped with blender, constant pressure funnel, condenser pipe and nitrogen conduit, using the method for polymerisation in solution, is delayed
Slow stirring is warming up to 70-80 DEG C, obtains polymer solution, and adding account for polymer solution 8-10% is in mass ratio 1:2 group
At zinc acetate and acid anhydrides mixed liquor, be to slowly warm up to acid anhydrides under nitrogen protection and when zinc acetate is completely dissolved, side stirring
While being warming up to 250-280 DEG C, insulation reaction 2-3h is cooled to 200-220 DEG C, obtains mixture B；
Step 3, in mass ratio 2:3:4:1:2 are by polyester resin, isocyanates, peach gum, mixture B and tri-methyl hexamethylene
Diamines is added in reaction kettle, and keeping temperature is 180-200 DEG C, is stirred to react 1-2h, is cooled to room temperature to obtain tackifying assistant；
Step 4 according to parts by weight helps the thickening of A, 15-20 parts of step 3 of the premix preparation in 50-60 parts of step 1
Agent, 5-10 parts of natural gum juice, 8-10 parts of diatomites in powder are added in blender, first carry out high-speed stirred 35- with 135-145r/min
45min is then added 3-5 parts of auxiliary agents, is stirred at low speed with 75-85r/min, stirs 45min to get environmental protection of the invention
The viscous adhesive of height.
2. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 1, which is characterized in that the nitration mixture is dense
The mixture that sulfuric acid, concentrated nitric acid are formed according to weight ratio 2:1.
3. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 1, which is characterized in that the hydroxypropyl forms sediment
Powder, preparation method thereof is that starch is added in reaction flask, and sodium sulphate, sodium hydroxide is then added, is filled with nitrogen, then adds
Propylene oxide stirs 15-25min, and then adding mass fraction is 50-60% dilute sulfuric acid, until solution is neutrality, then be centrifuged,
Washing, drying are to get hydroxypropul starch.
4. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 1, which is characterized in that layered secondary phosphorus
The preparation method of hydrochlorate is that aluminium chloride, sodium hypophosphite, Pluronic F68 are placed in autoclave, and nothing is added
Rare earth oxide, mica powder is then added in water-ethanol, stirring thereto again, carries out ultrasonic disperse 15-25min, is subsequently placed at baking
3.5h is handled in case, then is filtered, is washed, then is placed in baking oven dry, grinding as stratiform hypophosphites, finally by stratiform time phosphorus
Hydrochlorate carries out sided corona treatment 5-9min.
5. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 4, which is characterized in that the rare-earth oxidation
Object is cerium oxide.
6. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 4, which is characterized in that the sided corona treatment
Power is 5KW, and treatment temperature is 45 DEG C.
7. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 1, which is characterized in that the natural gum juice
The mixture formed for pin tree sap, Bajiao Banana Juice according to weight ratio 4:1.
8. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 1, which is characterized in that the diatomite in powder
For the high-quality diatomite ore of silica containing 90%, by calcining, calcination temperature is 850-950 DEG C, calcines 25min, then crush
It is sent into sorting machine and sorts.
9. a kind of preparation method of the high viscous adhesive of environmental protection according to claim 1, which is characterized in that the auxiliary agent is three
Polyphosphate sodium, lignin are mixed according to weight ratio 5:2.
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Application publication date: 20181221 |