CN109294459A - A kind of high-efficiency environment friendly adhesive and glued board - Google Patents
A kind of high-efficiency environment friendly adhesive and glued board Download PDFInfo
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- CN109294459A CN109294459A CN201811212912.XA CN201811212912A CN109294459A CN 109294459 A CN109294459 A CN 109294459A CN 201811212912 A CN201811212912 A CN 201811212912A CN 109294459 A CN109294459 A CN 109294459A
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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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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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Abstract
The invention discloses a kind of high-efficiency environment friendly adhesive and glued boards, it is related to adhesive technology field, this kind of adhesive includes following raw material: gelatinization green starch, coumarone indene resin, Faku County's clay, rectorite powder, neopentylglycol dimethacrylate, polyvinyl ethyl ether, diacetone acrylamide, phenyl dichloro phosphorus, compounding crosslinking agent, compounding coupling agent, Compound accelerator, compound antioxidant.Adhesive of the invention bonding strength, waterproofness, resistance to oxidation aging, in terms of on promoted significant, improve the overall performance of adhesive, improve application performance, service life is more secure, has good promotional value.
Description
Technical field
The present invention relates to adhesive technology fields, and in particular to a kind of high-efficiency environment friendly adhesive and glued board.
Background technique
Adhesive includes two class of Organic adhesive and inorganic adhesive, and Organic adhesive mainly has silicone resin, silicon rubber, gathers
Acid imide, phenolic aldehyde, epoxy resin etc., and inorganic adhesive mainly has silicates, alkali metal phosphate class and silica solution etc..Have
Machine adhesive huge number, generally higher for the adhesion strength of material, if epoxy adhesive is known as omnipotent adhesive, kind is many
It is more, it is widely used；Phenolic resin is earliest industrialized synthetic resin, as adhesive is big with bond strength, carbon residue is high
Advantage causes Organic adhesive commonly used in the viscous of organic material due to the incompatibility between organic material and inorganic material
Knot, and inorganic adhesive is then chiefly used in the bonding of inorganic material, limits respective development, utilizes inorganic adhesive and organic gel
The advantages of both sticks, researches and develops organic and inorganic composite type adhesive, is future developing trend.
Application No. is 201310059918.9 Chinese patents to disclose a kind of ornament materials adhesive, by following weight
The raw material of part is made: styrene 100-120, ethyl acetate 100-150, neoprene CR12120-25, dimethylbenzene 15-20,4,
4 '-methyl diphenylene diisocyanate 1-2, polyisobutene 8-12,3- aminopropyl trimethoxysilane 2-3, polytetrahydrofuran ether
Glycol 2-3, SG-2 type polyvinyl chloride resin 3-5, ferrocene 1-2, chlorohydrin rubber H758-12, butadiene-styrene rubber 5-8, zinc oxide 2-3 etc..It should
Kind adhesive is heat-resisting water-fast, and adhesion strength is high, but its freeze-thaw resistance is poor, and application is restricted.
Application No. is 201711231179.1 Chinese patents to disclose a kind of floor adhesive, this kind of adhesive includes
The raw material of following parts by weight: 10~15 parts of butyl acrylate, 30~40 parts of vinyl acetate resin, precipitated calcium carbonate 20~30
It is part, 5~10 parts of flake asbestos, 30~40 parts of ethyl alcohol, 0.03~0.05 part of ultraviolet absorbing agent, 0.1~0.2 part of antioxidant, fire-retardant
0.2~0.3 part of agent, 40~50 parts of deionized water.The waterproof and dampproof property of this kind of adhesive is good, but its heat aging is poor, application
Property is restricted.
Summary of the invention
The purpose of the present invention is to provide a kind of high-efficiency environment friendly adhesive and glued board, this kind of adhesive overall performance is excellent
More, problems of the prior art can be well solved.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of high-efficiency environment friendly adhesive is made of following raw material according to parts by weight:
Green starch 64-72 parts of gelatinization；
27-32 parts of coumarone indene resin；
Clay 6-9 parts of Faku County；
9-12 parts of rectorite powder；
4-5.5 parts of neopentylglycol dimethacrylate；
2-3 parts of polyvinyl ethyl ether；
3-4.5 parts of diacetone acrylamide；
1.5-2.2 parts of phenyl dichloro phosphorus；
Crosslinking agent 2.8-3.7 parts of compounding；
Coupling agent 1-1.7 parts of compounding；
0.8-1.1 parts of Compound accelerator；
1-1.6 parts of compound antioxidant；
Above-mentioned Compound accelerator be captax, two kinds of ingredients of Vulcanization accelerator TMTD according to mass ratio be (4-5.5): (3-4.5)
What merging obtained.
Further, above-mentioned compound antioxidant be antioxidant DLTDP, antioxidant 1076, three kinds of ingredients of irgasfos 168 according to
Mass ratio (1-2.5): (2-3.5): (2-2.8) merging obtains.
Further, above-mentioned adhesive is made of following raw material according to parts by weight:
72 parts of green starch of gelatinization；
32 parts of coumarone indene resin；
9 parts of Faku County's clay；
12 parts of rectorite powder；
5.5 parts of neopentylglycol dimethacrylate；
3 parts of polyvinyl ethyl ether；
4.5 parts of diacetone acrylamide；
2.2 parts of phenyl dichloro phosphorus；
3.7 parts of crosslinking agent of compounding；
1.7 parts of coupling agent of compounding；
1.1 parts of Compound accelerator；
1.6 parts of compound antioxidant.
Further, above-mentioned gelatinization green starch preparation method is as follows:
First weigh 50 parts of green starch, 25 parts of polyvinyl alcohol, 70 parts of water；Again at room temperature by green starch, polyvinyl alcohol, water
It mixes, is again heated to 81 DEG C and is gelatinized, the product after gelatinization is placed in 60Co- gamma Rays field radiates later
Graft polymerization, and dose of radiation is 1.8kGy, dosage rate 0.26kGy/h.
Further, above-mentioned compounding crosslinking agent is that two kinds of amino resins, crosslinking aid S aC-100 ingredients are according to mass ratio
What 2.7:1.8 merging obtained.
Further, above-mentioned compounding coupling agent is silane coupling A -151, two kinds of ingredients of anti-settling Aluminate ASA are pressed
It is what 4.5:2.5 merged according to mass ratio.
Further, it according to mass ratio is 5.5 that above-mentioned Compound accelerator, which is two kinds of captax, Vulcanization accelerator TMTD ingredients:
What 4.5 merging obtained.
Further, above-mentioned compound antioxidant be antioxidant DLTDP, antioxidant 1076, three kinds of ingredients of irgasfos 168 according to
Mass ratio is what 2.5:3.5:2.8 merged.
Further, above-mentioned adhesive the preparation method is as follows:
Step 1: weighing raw material by above-mentioned parts by weight, follow the example of library clay and rectorite powder combination drying, and be milled to thin
Degree 35 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 38% is first added, which dilutes, to be mixed, and is again heated to 47 DEG C, is added
5.5min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 4.5min obtains mixing A under the conditions of degree is 49 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 11min under the conditions of 58 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 15min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed to obtain mixing C in material B, mixing C is delivered in colloid mill equipment the decentralized processing 4.5min that mills later, it is described
Engine speed is 3500rpm in colloid mill equipment, and operating temperature is 58 DEG C, operating pressure 9bar.
A kind of glued board is made of the plank layer, adhesive layer, plank layer, adhesive layer and the plank layer that set gradually, and
Adhesive layer is that above-mentioned adhesive is coated with.
The present invention have it is following the utility model has the advantages that in the present invention Faku County's clay, rectorite powder, polyvinyl ethyl ether etc. at
The addition divided can be improved the surface molecular activity of gelatinization green starch, can effectively be connected with coumarone indene resin molecule
It connects, forms three-dimensional molecular reticular structure, the bonding strength for the adhesive layer being formed by curing is significantly improved, the knot between molecule
Resultant force is significantly enhanced, and the erosion of the extraneous factors such as light, heat, cold, oxygen gas and water is small to the destruction of its chemical bond, from
And ageing-resistant performance, hydrophobicity, temperature tolerance, frost resistance of adhesive layer etc. can be further improved, and this kind of composite adhesive
Simple and convenient, environmentally protective, formaldehydeless pollution, nonhazardous, and the glue-line flame-proof antibiotic being formed by curing are prepared, application performance is good,
Application field is extensive.
Specific embodiment
Below with reference to embodiment, further description of the specific embodiments of the present invention, and following embodiment is only used for more
Technical solution of the present invention is clearly demonstrated, and not intended to limit the protection scope of the present invention.
It all raw materials in embodiment and its produces composition and can be obtained by disclosed commercially available channel；
Embodiment 1
The present embodiment is related to a kind of high-efficiency environment friendly adhesive, this kind of adhesive is by following raw material group according to parts by weight
At:
64 parts of green starch of gelatinization；
27 parts of coumarone indene resin；
6 parts of Faku County's clay；
9 parts of rectorite powder；
4 parts of neopentylglycol dimethacrylate；
2 parts of polyvinyl ethyl ether；
3 parts of diacetone acrylamide；
1.5 parts of phenyl dichloro phosphorus；
2.8 parts of crosslinking agent of compounding；
1 part of coupling agent of compounding；
0.8 part of Compound accelerator；
1 part of compound antioxidant.
It is gelatinized the selection of green starch, compounding crosslinking agent, compounding coupling agent and compound antioxidant in the present embodiment and produces
It is as shown in table 1 below:
Table 1
The preparation method of adhesive substantially follows the steps below in the present embodiment:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 20 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 30% is first added, which dilutes, to be mixed, and is again heated to 44 DEG C, is added
7min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 6min obtains mixing A under the conditions of being 46 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 15min under the conditions of 55 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 12min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed to obtain mixing C in material B, mixing C is delivered in CM2000-4 type colloid mill equipment the decentralized processing 3min that mills later
Adhesive is got product, engine speed is 5000rpm in above-mentioned colloid mill equipment, and operating temperature is 65 DEG C, and operating pressure is
12bar。
Embodiment 2
The present embodiment is related to a kind of high-efficiency environment friendly adhesive, this kind of adhesive is by following raw material group according to parts by weight
At:
68 parts of green starch of gelatinization；
30 parts of coumarone indene resin；
7 parts of Faku County's clay；
10 parts of rectorite powder；
4.5 parts of neopentylglycol dimethacrylate；
2.5 parts of polyvinyl ethyl ether；
3.5 parts of diacetone acrylamide；
1.8 parts of phenyl dichloro phosphorus；
3.3 parts of crosslinking agent of compounding；
1.3 parts of coupling agent of compounding；
0.9 part of Compound accelerator；
1.4 parts of compound antioxidant.
It is gelatinized the selection of green starch, compounding crosslinking agent, compounding coupling agent and compound antioxidant in the present embodiment and produces
It is as shown in table 2 below:
Table 2
The preparation method of adhesive substantially follows the steps below in the present embodiment:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 25 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 32% is first added, which dilutes, to be mixed, and is again heated to 45 DEG C, is added
6.5min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 5.5min obtains mixing A under the conditions of degree is 47 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 14min under the conditions of 56 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 13min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed to obtain mixing C in material B, mixing C is delivered in CM2000-4 type colloid mill equipment decentralized processing of milling later
3.5min gets product adhesive, and engine speed is 4500rpm in above-mentioned colloid mill equipment, and operating temperature is 62 DEG C, work pressure
Power is 11bar.
Embodiment 3
The present embodiment is related to a kind of high-efficiency environment friendly adhesive, this kind of adhesive is by following raw material group according to parts by weight
At:
70 parts of green starch of gelatinization；
31 parts of coumarone indene resin；
8 parts of Faku County's clay；
11 parts of rectorite powder；
5 parts of neopentylglycol dimethacrylate；
2.8 parts of polyvinyl ethyl ether；
4 parts of diacetone acrylamide；
2 parts of phenyl dichloro phosphorus；
3.5 parts of crosslinking agent of compounding；
1.5 parts of coupling agent of compounding；
1 part of Compound accelerator；
1.5 parts of compound antioxidant.
It is gelatinized the selection of green starch, compounding crosslinking agent, compounding coupling agent and compound antioxidant in the present embodiment and produces
It is as shown in table 3 below:
Table 3
The preparation method of adhesive substantially follows the steps below in the present embodiment:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 30 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 35% is first added, which dilutes, to be mixed, and is again heated to 46 DEG C, is added
6min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 5min obtains mixing A under the conditions of being 48 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 12min under the conditions of 57 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 14min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed to obtain mixing C in material B, mixing C is delivered in CM2000-4 type colloid mill equipment the decentralized processing 4min that mills later
Adhesive is got product, engine speed is 4000rpm in above-mentioned colloid mill equipment, and operating temperature is 60 DEG C, and operating pressure is
10bar。
Embodiment 4
The present embodiment is related to a kind of high-efficiency environment friendly adhesive, this kind of adhesive is by following raw material group according to parts by weight
At:
72 parts of green starch of gelatinization；
32 parts of coumarone indene resin；
9 parts of Faku County's clay；
12 parts of rectorite powder；
5.5 parts of neopentylglycol dimethacrylate；
3 parts of polyvinyl ethyl ether；
4.5 parts of diacetone acrylamide；
2.2 parts of phenyl dichloro phosphorus；
3.7 parts of crosslinking agent of compounding；
1.7 parts of coupling agent of compounding；
1.1 parts of Compound accelerator；
1.6 parts of compound antioxidant.
It is gelatinized the selection of green starch, compounding crosslinking agent, compounding coupling agent and compound antioxidant in the present embodiment and produces
It is as shown in table 4 below:
Table 4
The preparation method of adhesive substantially follows the steps below in the present embodiment:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 35 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 38% is first added, which dilutes, to be mixed, and is again heated to 47 DEG C, is added
5.5min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 4.5min obtains mixing A under the conditions of degree is 49 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 11min under the conditions of 58 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 15min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed to obtain mixing C in material B, mixing C is delivered in CM2000-4 type colloid mill equipment decentralized processing of milling later
4.5min gets product adhesive, and engine speed is 3500rpm in above-mentioned colloid mill equipment, and operating temperature is 58 DEG C, work pressure
Power is 9bar.
Embodiment 5
The present embodiment is related to a kind of high-efficiency environment friendly adhesive, this kind of adhesive is by following raw material group according to parts by weight
At:
78 parts of green starch of gelatinization；
35 parts of coumarone indene resin；
10 parts of Faku County's clay；
13 parts of rectorite powder；
6 parts of neopentylglycol dimethacrylate；
3.5 parts of polyvinyl ethyl ether；
5 parts of diacetone acrylamide；
2.5 parts of phenyl dichloro phosphorus；
4.2 parts of crosslinking agent of compounding；
2 parts of coupling agent of compounding；
1.2 parts of Compound accelerator；
2 parts of compound antioxidant.
It is gelatinized the selection of green starch, compounding crosslinking agent, compounding coupling agent and compound antioxidant in the present embodiment and produces
It is as shown in table 5 below:
Table 5
The preparation method of adhesive substantially follows the steps below in the present embodiment:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 40 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 40% is first added, which dilutes, to be mixed, and is again heated to 48 DEG C, is added
5min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 4min obtains mixing A under the conditions of being 50 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 10min under the conditions of 59 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 16min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed to obtain mixing C in material B, mixing C is delivered in CM2000-4 type colloid mill equipment the decentralized processing 5min that mills later
Adhesive is got product, engine speed is 3000rpm in above-mentioned colloid mill equipment, and operating temperature is 55 DEG C, and operating pressure is
8bar。
Comparative example group
"-" indicates that the reduction of certain ingredient in embodiment uses in the following table 6；
Table 6
Comparative example 8
This comparative example is related to a kind of adhesive, and relative to above-described embodiment 1, there is only the ingredient of crosslinking agent differences；
The ingredient of this comparative example crosslinking agent are as follows: amino resins.
Comparative example 9
This comparative example is related to a kind of adhesive, and relative to above-described embodiment 2, there is only coupling agent mass ratio of each components
It is different；
This comparative example coupling agent mass ratio of each component are as follows: silane coupling A -151: anti-settling Aluminate ASA=1:1.
Comparative example 10
This comparative example is related to a kind of adhesive, and relative to above-described embodiment 3, there is only the ingredient of promotor differences；
The ingredient of this comparative example promotor are as follows: captax.
Comparative example 11
This comparative example is related to a kind of adhesive, and relative to above-described embodiment 4, there is only antioxidant mass ratio of each components
It is different；
This comparative example antioxidant mass ratio of each component are as follows: antioxidant DLTDP: antioxidant 1076: irgasfos 168=1:1:1.
Comparative example 12
This comparative example is related to a kind of adhesive, and relative to above-described embodiment 5, there is only the preparation methods of adhesive not
Together；
This comparative example adhesive the preparation method is as follows:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 40 μm filler it is stand-by；
Step 2: 30min is mixed under the conditions of temperature is 46 DEG C in all raw materials jointly, the mixing that will be obtained later
It is delivered in CM2000-4 type colloid mill equipment the decentralized processing 5min that mills and gets product adhesive, master in above-mentioned colloid mill equipment
Machine revolving speed is 3000rpm, and operating temperature is 55 DEG C, operating pressure 8bar.
Comparative example 13
This comparative example is related to a kind of adhesive, and relative to above-described embodiment 5, there is only the preparation methods of adhesive not
Together；
This comparative example adhesive the preparation method is as follows:
Step 1: weighing above-mentioned raw materials according to parts by weight；Follow the example of library clay and rectorite powder combination drying, and ball milling
To fineness 40 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 40% is first added, which dilutes, to be mixed, and is again heated to 48 DEG C, is added
5min is mixed in coumarone indene resin and diacetone acrylamide, under the conditions of being subsequently agitated for, pours into polyvinyl ethyl ether in temperature
Insulated and stirred 4min obtains mixing A under the conditions of being 50 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be in temperature
After keeping the temperature 10min under the conditions of 59 DEG C, under stirring condition, sequentially adds filler, compounding coupling agent and Compound accelerator and continue
Stirring 16min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mix under agitation
It is sufficiently mixed in material B and gets product adhesive.
Comparative example 14
Application No. is a kind of floor adhesives disclosed in 201711231179.1.
Performance detection
Following performance detection, testing result note are carried out to adhesive made from above-described embodiment 1-5 and comparative example 1-14
Record in table 7 that (the adhesive detection material of embodiment 1-5 indicates that the adhesive of comparative example 1-14 detection material is adopted using #1-#5 in table
It is indicated with &1-&14)
Detection test specimen is produced: being taken birch lumber, is spread embodiment 1-5 and comparative example 1-14 respectively at a surface thereof and be made
Adhesive detect material, sizing solid content be 15g/m2, take other one piece of birch lumber and sizing face paste to close after drying again, warp
After press machine (operating pressure 2.0MPa, compacting time are 10min) compacting bonding, by the double-deck birch plywood after standing 12h
The sheet material having a size of 5 × 5cm is cut into as detection test specimen.
It is as follows that properties detect general steps:
(1) bonding strength: under standard test conditions, 10 test piece maintenance 5d is taken, after maintenance, test specimen is put into
It in tensile shear testing fixture, is loaded with the speed of 10mm/min, until test specimen destroys, measures bonding strength, take its average value.
(2) under standard test conditions, by 10 test piece maintenance 5d, (23 ± 2) bonding strength after soaking: are then immersed in
DEG C water in 7d, test specimen is taken out, is dried with a cloth, measure bonding strength, take its average value.
(3) bonding strength after heat ageing: under standard test conditions, then test specimen is put by 10 test piece maintenance 5d
7d in (60 ± 2) DEG C convection oven.Guarantee that each test specimen surrounding air freely recycles.Test specimen taking-up is put in normal conditions again
It sets for 24 hours, measures bonding strength, take its average value.
(4) bonding strength after high/low temperature alternative cycle: under standard test conditions, by 10 test piece maintenance 5d.Then it soaks
Enter 30min in the water of (15 ± 2) DEG C, then be placed on 30min in 80 DEG C of water, is repeated 4 times circulation.Test specimen is placed on to be cooled down at room temperature
After 30min, bonding strength is measured, its average value is taken.
(5) bonding strength after Frozen-thawed cycled: under standard test conditions, by 10 test piece maintenance 5d.Then (23 ±
DEG C 2) 4h ± 20min is impregnated in water, is placed on (- 20 ± 3) DEG C cryogenic box and is frozen 4h ± 20min, then puts in the water of people (23 ± 2) DEG C
4h is impregnated, repeatedly 30 circulations.It takes out test specimen and places 4h at room temperature, measure bonding strength, take its average value.
Table 7
Adhesive of the invention is in bonding strength, waterproofness, resistance to oxidation aging, temperature tolerance etc. it can be seen from upper table 7
It is promoted significantly on aspect of performance, is improved compared to existing adhesive overall performance, improves application performance, service life
It is more secure, there is good promotional value.
In conjunction with the beneficial effect of the present invention, applicant illustrates constituent part and preparation method of the invention as follows:
(1) compound crosslinking agent: the type of crosslinking agent applied to high molecular material is various, is suitable for the present invention to search out
The crosslinking agent of adhesive system, applicant through a large number of experiments, surprisingly obtain by amino resins, crosslinking aid S aC-100 two
Kind ingredient is (2-3) in mass ratio: (1-2) merges obtained compounding crosslinking agent, this kind of crosslinking agent can preferably realize this hair
Bright beneficial effect and purpose can make quickly to form a large amount of and distribution between framework strand in adhesive of the present invention
Even bridged bond, the 3 D stereo reticular structure being built into is form compact and stable, and the synergistic effect of the other raw materials of compatibility can be mentioned preferably
The overall performance of high adhesive.If compounding the ingredient of crosslinking agent or/and the change of content in the present invention, the present invention will lead to
Beneficial effect cannot realize well.
(2) compound coupling agent: the common coupling agent of adhesive is mostly silane series coupling agent, is used for organic polymer
It reacts and merges with inorganic filler, show that silane coupling A -151 is being applied in many silane series coupling agent products through research
The effect generated in the present invention is best, but expected requirement is not achieved, and therefore, applicant attempts to add the idol of other ingredients
Connection agent merges with it using and then come reach the purpose of the present invention, and on this basis, applicant finally surprisingly obtains silane idol
Two kinds of connection agent A-151, anti-settling Aluminate ASA ingredients are (3-5) according to mass ratio: (1-3) merges obtained compounding and is coupled
Agent, this kind compounds the beneficial effect that coupling agent obtains and protrudes very much, considerably beyond other types and the coupling agent assembled, Neng Gougao
The ingredients such as Faku County's clay, rectorite powder are filled in effect ground adhesion promotion raw material is coated into polymeric matrix, is mentioned significantly
The ability that high adhesive material interface is damaged from environmental stress.If compounding the ingredient of coupling agent in the present invention or/and containing
The change of amount, will lead to beneficial effects of the present invention cannot realize well.
(3) Compound accelerator: use two kinds of captax, Vulcanization accelerator TMTD ingredients according to mass ratio for (4-6): (3-5)
Merging obtained mixed type promotor is more suitable for adhesive material system of the invention, and the two synergistic effect can greatly improve
Reaction promotes efficiency, is effectively improved the comprehensive performance of adhesive；If the composition of promotor or/and content changes in the present invention
Become, will lead to beneficial effects of the present invention cannot realize well.
(4) compound antioxidant: finding through applicant's many experiments, antioxidant DLTDP, antioxidant 1076, irgasfos 168
The synergistic effect of three kinds of ingredients can effectively prevent the progress of adhesive chain reaction of the present invention, both can be reduced the use of antioxidant
Antioxygen can be improved prevents old effect to amount again, very helpful to the service life for extending adhesive of the present invention；If being compounded in the present invention
The ingredient of antioxidant or/and the change of content, will lead to beneficial effects of the present invention cannot realize well.
Certainly, because of the requirement of the mentality of designing and goal of the invention of adhesive of the present invention, remaining of the invention component selection and
Content selection is obviously also non-obvious, and those skilled in the art combine the prior art that can readily occur in absolutely not.This
Have further embodiment in the preparation method of adhesive of the present invention, in conjunction with the embodiment of the present invention it can be seen that, system of the invention
Preparation Method is designed using four steps, and raw material is added in mixing process by several times in batches, and step is simple and orderly, rather than is used existing
Technology is conventional to be added at one time (such as comparative example 12), and this technique is the special proportion phase with adhesive raw materials for production component
It adapts to, only uses this technique, just can guarantee that the smooth sequential of adhesive reaction system carries out, what guarantee was finally prepared
Adhesive excellent characteristics.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of high-efficiency environment friendly adhesive, which is characterized in that be made of following raw material according to parts by weight:
Green starch 64-72 parts of gelatinization；
27-32 parts of coumarone indene resin；
Clay 6-9 parts of Faku County；
9-12 parts of rectorite powder；
4-5.5 parts of neopentylglycol dimethacrylate；
2-3 parts of polyvinyl ethyl ether；
3-4.5 parts of diacetone acrylamide；
1.5-2.2 parts of phenyl dichloro phosphorus；
Crosslinking agent 2.8-3.7 parts of compounding；
Coupling agent 1-1.7 parts of compounding；
0.8-1.1 parts of Compound accelerator；
1-1.6 parts of compound antioxidant；
The Compound accelerator be captax, two kinds of ingredients of Vulcanization accelerator TMTD according to mass ratio be (4-5.5): (3-4.5) merge
It obtains.
2. a kind of high-efficiency environment friendly adhesive according to claim 1, which is characterized in that the compound antioxidant is antioxidant
Three kinds of DLTDP, antioxidant 1076, irgasfos 168 ingredients are (1-2.5): (2-3.5) according to mass ratio: (2-2.8) merging obtains
's.
3. a kind of high-efficiency environment friendly adhesive according to claim 1, which is characterized in that by following original according to parts by weight
Material composition:
72 parts of green starch of gelatinization；
32 parts of coumarone indene resin；
9 parts of Faku County's clay；
12 parts of rectorite powder；
5.5 parts of neopentylglycol dimethacrylate；
3 parts of polyvinyl ethyl ether；
4.5 parts of diacetone acrylamide；
2.2 parts of phenyl dichloro phosphorus；
3.7 parts of crosslinking agent of compounding；
1.7 parts of coupling agent of compounding；
1.1 parts of Compound accelerator；
1.6 parts of compound antioxidant.
4. a kind of high-efficiency environment friendly adhesive according to claim 3, which is characterized in that the gelatinization green starch side of producing
Method is as follows:
First weigh 50 parts of green starch, 25 parts of polyvinyl alcohol, 70 parts of water；Green starch, polyvinyl alcohol, water are mixed at room temperature again
It is even, be again heated to 81 DEG C and be gelatinized, the product after gelatinization is placed in 60Co- gamma Rays field later carry out radiation connect
Branch polymerization, and dose of radiation is 1.8kGy, dosage rate 0.26kGy/h.
5. a kind of high-efficiency environment friendly adhesive according to claim 4, which is characterized in that the compounding crosslinking agent is amino tree
Two kinds of rouge, crosslinking aid S aC-100 ingredients are what 2.7:1.8 merged according to mass ratio.
6. a kind of high-efficiency environment friendly adhesive according to claim 5, which is characterized in that the compounding coupling agent is that silane is even
Two kinds of connection agent A-151, anti-settling Aluminate ASA ingredients are what 4.5:2.5 merged according to mass ratio.
7. a kind of high-efficiency environment friendly adhesive according to claim 6, which is characterized in that the Compound accelerator is promotor
M, two kinds of ingredients of Vulcanization accelerator TMTD are what 5.5:4.5 merged according to mass ratio.
8. a kind of high-efficiency environment friendly adhesive according to claim 7, which is characterized in that the compound antioxidant is antioxidant
Three kinds of DLTDP, antioxidant 1076, irgasfos 168 ingredients are what 2.5:3.5:2.8 merged according to mass ratio.
9. a kind of high-efficiency environment friendly adhesive according to claim 8, which is characterized in that the preparation method of the adhesive is such as
Under:
Step 1: weighing raw material by the parts by weight, follow the example of library clay and rectorite powder combination drying, and be milled to fineness and exist
35 μm filler it is stand-by；
Step 2: taking gelatinization green starch, the water that starch weight 38% is first added, which dilutes, to be mixed, and is again heated to 47 DEG C, and ancient horse is added
5.5min is mixed in grand resin and diacetone acrylamide, and under the conditions of being subsequently agitated for, pouring into polyvinyl ethyl ether in temperature is
Insulated and stirred 4.5min obtains mixing A under the conditions of 49 DEG C；
Step 3: taking neopentylglycol dimethacrylate to be poured slowly into mixing A and be sufficiently mixed stirring, be 58 DEG C in temperature
Under the conditions of keep the temperature 11min after, under stirring condition, sequentially add filler, compounding coupling agent and Compound accelerator persistently stir
15min obtains mixed material B；
Step 4: phenyl dichloro phosphorus, compound antioxidant and compounding crosslinking agent being taken to be added sequentially to mixed material B under agitation
In be sufficiently mixed to obtain mixing C, mixing C is delivered in colloid mill equipment the decentralized processing 4.5min that mills, the glue later
It is 3500rpm that body, which grinds engine speed in equipment, and operating temperature is 58 DEG C, operating pressure 9bar.
10. a kind of glued board is made of the plank layer, adhesive layer, plank layer, adhesive layer and the plank layer that set gradually,
It is characterized in that, the adhesive layer is that the described in any item adhesives of claim 1-9 are coated with.
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| CN201811212912.XA CN109294459A (en) | 2018-10-18 | 2018-10-18 | A kind of high-efficiency environment friendly adhesive and glued board |
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