CN109021872A - A kind of fire-retardant high viscous environmental protection type sealing adhesive - Google Patents
A kind of fire-retardant high viscous environmental protection type sealing adhesive Download PDFInfo
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- CN109021872A CN109021872A CN201810717789.0A CN201810717789A CN109021872A CN 109021872 A CN109021872 A CN 109021872A CN 201810717789 A CN201810717789 A CN 201810717789A CN 109021872 A CN109021872 A CN 109021872A
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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
- C09J127/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Adhesives based on derivatives of such polymers
- C09J127/02—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J127/04—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Adhesives based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C09J127/06—Homopolymers or copolymers of vinyl chloride
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a kind of fire-retardant high viscous environmental protection type sealing adhesives, it is related to building sealant technical field, including following raw material: vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin, 20-30 μm of partial size of illite powder, methylisothiazolinone, 15-30 μm of partial size of villus powder, triphenylmethane triisocyanate, flaxseed gum, tricresyl phosphate (butoxyethyl group) ester, dispersing agent FT-78, crosslinking agent, promotor, antioxidant, coupling agent.Sealant of the invention prepares simple and convenient, and surface drying speed is fast, and glue-line cross-linked structure is form compact and stable, and stretch-bonded performance is good, and fire-retardant high-low temperature resistant, water-proof climate resisting, heat preservation and soundproof, expelling parasite antifungi, energy-saving and environment friendly, application field is extensive, long service life.
Description
Technical field
The present invention relates to building sealant technical fields, and in particular to a kind of fire-retardant high viscous environmental protection type sealing adhesive.
Background technique
Common building sealant is mostly polyurethane sealant and silicon rubber sealant both at home and abroad at present.Polyurethane
Sealant production technology is complicated, and equipment requirement is high, and investment is big, and due to utilizing moisture-curable principle, polyurethane sealant storage
Deposit stablize it is poor, if closed slightly not tight or temperature is slightly higher, easily solidification failure.Polyurethane sealant to vinyl material such as
The common building materials bonding force such as PVC, EVA, PE is weak, and adhesive strength does not often reach requirement.In addition, due to polyurethane seal glue residua
Isocyanates be harmful to the human body, therefore not environmentally, weatherability is also poor.Silicone rubber kinds sealant has a wide range of application, but silicon rubber
Acetic acid can be released when class sealing glue solidifying, acetic acid not only has strong impulse stink, can pollute air, can also be to metal
Corrosiveness is generated, and does not have after being fully cured and holds viscous function, therefore, it is necessary to develop go out a kind of novel, environmentally friendly, property
It can excellent, comprehensive fluid sealant for construction.
The patent application of Publication No. CN107541174A discloses a kind of monocomponent polyurethane building sealant, this kind
Sealant is calculated according to weight percent, including following components: polyurethane prepolymer A and polyurethane prepolymer B totally 35~55%,
Silane coupling agent 1~3%, modified coal ash 5~10%, latent curative 0.5~0.8%, dicyclopentadiene petroleum resin 10
~20%, plasticizer 10~20%, filler 10~30%, ultraviolet absorbing agent and stabilizer 0.1~3%.This kind of sealant tool
There are good good weatherability and waterproofness, but its cementability is poor, application is affected.
The patent application for authorizing Publication No. CN102838964B, discloses a kind of High-weather-fastnespolysulfide polysulfide sealant, including
Base cream and vulcanization cream, base cream includes weight percent 30-70% liquid polysulfide glue, 20-60% filler, 1-10% tackifier, 3-
20% plasticizer, 0.3-5% coupling agent, 0.1-2% antioxidant and 0.05-1% UV resistance agent;Vulcanizing cream includes 25-70% sulphur
Agent, 25-70% plasticizer and 0.5-5% vulcanization accelerator.This kind of sealant is improved using antioxidant and UV resistance agent
The weatherability of sealant, with good stability and reproducibility, but its anti-flammability is poor, application is affected.
Summary of the invention
The purpose of the present invention is to provide a kind of fire-retardant high viscous environmental protection type sealing adhesive, this kind seals plastic structure cross-linked stable and causes
It is close, high comprehensive performance.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of fire-retardant high viscous environmental protection type sealing adhesive, is made of following raw material by weight:
52 parts of vinyl chloride-acrylate copolymer;
40 parts of tertiary butyl phenol aldehyde tackifying resin;
14 parts of 30 μm of partial size of illite powder;
5 parts of methylisothiazolinone;
11 parts of 30 μm of partial size of villus powder;
8 parts of triphenylmethane triisocyanate;
5 parts of flaxseed gum;
6 parts of ester of tricresyl phosphate (butoxyethyl group);
FT-781.2 parts of dispersing agent;
5 parts of crosslinking agent;
1.5 parts of promotor;
2.5 parts of antioxidant;
0.6 part of coupling agent.
Further, above-mentioned sealant the preparation method is as follows:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add phase
When the glycerine of the weight of material 12% in reaction kettle, reaction 4min, Zhi Houjia are mixed under conditions of temperature is 65 DEG C
Heat is warming up to 80 DEG C, and triphenylmethane triisocyanate is added and reaction 3min is mixed in promotor, obtains mixing A;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 80 DEG C, vacuum degree is
Reaction 3min is mixed under conditions of 0.06MPa, adds tricresyl phosphate (butoxyethyl group) ester later and dispersing agent FT-78 is protected
Reaction 2min is mixed in pressure heat preservation, obtains mixed material B;
Step 3: take mixing A and mixed material B to be added in reaction kettle jointly, first temperature be 90 DEG C, vacuum degree 0.03MPa
Under conditions of be mixed reaction 5min, add illite powder, villus powder and coupling agent later and continues to mix and be stirred to react
10min, is eventually adding antioxidant and reaction 3min is mixed in crosslinking agent.
Further, the speed of agitator of aforesaid reaction vessel is controlled in 300-400r/min.
Preferably, above-mentioned crosslinking agent is two kinds of Triallyl isocyanurate, polyethyleneglycol diacrylate compositions merging
It obtains.
Further, above-mentioned crosslinking agent is Triallyl isocyanurate, polyethyleneglycol diacrylate according to mass ratio
What 2:3 merged.
Preferably, above-mentioned coupling agent is gamma-aminopropyl-triethoxy-silane, two kinds of compositions of rare-earth coupling agent merge to obtain
's.
Further, above-mentioned coupling agent is gamma-aminopropyl-triethoxy-silane, rare-earth coupling agent according to mass ratio 5:2 conjunction
And obtain.
Further, above-mentioned promotor is tetramethyl thiourea, accelerant C hartwellB-515.71W according to mass ratio 2:3
What merging obtained.
Further, above-mentioned antioxidant is antioxidant 1010, irgasfos 168 according to mass ratio (3-5): (2-3) merges
It arrives.
Further, above-mentioned antioxidant is antioxidant 1010, irgasfos 168 merges according to mass ratio 5:3.
The present invention have it is following the utility model has the advantages that environmental protection type sealing adhesive of the invention by ingenious selection to raw materials for production and
The inventive improvements of its preparation process, vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin, illite powder in raw material
The collaboration of the compositions such as end, methylisothiazolinone, triphenylmethane triisocyanate interacts, and forms three-dimensional cross-linked densification
Stable structure, has following characteristics:
(1) surface drying speed is fast, and elastic recovery is excellent, and stretch-bonded performance is good, and displacement capacity is strong, good fluidity, fracture
Elongation is big;
(2) heat resistance is good, water-proof climate resisting, will not influence the caking property of sealant under high/low temperature and wet face state, fire-retardant
Grade is high, and flame retardant property complies fully with the requirement of FV-0 rank;
(3) heat preservation and soundproof is good, expelling parasite antifungi, and insulate antistatic, functional;
(4) product is fine and smooth, uniform viscous body, bubble-free, agglomeration, skinning, gelatin phenomenon, without being not easy to be dispersed to precipitate object,
It is easy to use, and nonirritant gas generates, energy-saving and environment friendly, good, the high production efficiency of materials compatibility energy, using effect
Good, application field occasion is extensive, long service life.
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 fire-retardant high viscous environmental protection type sealing adhesive and preparation method thereof, the sealant by it is following by weight
The raw material of meter forms:
46 parts of vinyl chloride-acrylate copolymer;
30 parts of tertiary butyl phenol aldehyde tackifying resin;
8 parts of 20 μm of partial size of illite powder;
3 parts of methylisothiazolinone;
7 parts of 15 μm of partial size of villus powder;
5.5 parts of triphenylmethane triisocyanate;
3 parts of flaxseed gum;
4 parts of ester of tricresyl phosphate (butoxyethyl group);
FT-780.8 parts of dispersing agent;
3 parts of crosslinking agent;
1 part of promotor;
1.5 parts of antioxidant;
0.4 part of coupling agent.
The selection of crosslinking agent, coupling agent, promotor, antioxidant obtains as shown in table 1 below in above-mentioned raw materials:
Table 1
The preparation method of above-mentioned sealant substantially follows the steps below:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add phase
When the glycerine of the weight of material 8% in reaction kettle, reaction 6min is mixed under conditions of temperature is 55 DEG C, heats later
70 DEG C are warming up to, triphenylmethane triisocyanate is added and reaction 5min is mixed in promotor, obtains mixing A;In the step
The speed of agitator of reaction kettle is 200r/min;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 70 DEG C, vacuum degree is
Reaction 5min is mixed under conditions of 0.04MPa, adds tricresyl phosphate (butoxyethyl group) ester later and dispersing agent FT-78 is protected
Reaction 4min is mixed in pressure heat preservation, obtains mixed material B;The speed of agitator of reaction kettle is 200r/min in the step;
Step 3: take mixing A and mixed material B to be added in reaction kettle jointly, first temperature be 80 DEG C, vacuum degree 0.01MPa
Under conditions of be mixed reaction 7min, add illite powder, villus powder and coupling agent later and continues to mix and be stirred to react
15min, is eventually adding antioxidant and reaction 5min is mixed in crosslinking agent, and the speed of agitator of reaction kettle is in the step
300r/min。
Embodiment 2
The present embodiment is related to a kind of fire-retardant high viscous environmental protection type sealing adhesive and preparation method thereof, the sealant by it is following by weight
The raw material of meter forms:
48 parts of vinyl chloride-acrylate copolymer;
34 parts of tertiary butyl phenol aldehyde tackifying resin;
10 parts of 20 μm of partial size of illite powder;
3.5 parts of methylisothiazolinone;
8 parts of 15 μm of partial size of villus powder;
6.5 parts of triphenylmethane triisocyanate;
3.5 parts of flaxseed gum;
4.5 parts of ester of tricresyl phosphate (butoxyethyl group);
FT-780.9 parts of dispersing agent;
3.5 parts of crosslinking agent;
1.2 parts of promotor;
1.8 parts of antioxidant;
0.45 part of coupling agent.
The selection of crosslinking agent, coupling agent, promotor, antioxidant obtains as shown in table 2 below in above-mentioned raw materials:
Table 2
The preparation method of above-mentioned sealant substantially follows the steps below:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add phase
When the glycerine of the weight of material 9% in reaction kettle, reaction 5.5min, Zhi Houjia are mixed under conditions of temperature is 58 DEG C
Heat is warming up to 72 DEG C, and triphenylmethane triisocyanate is added and reaction 4.5min is mixed in promotor, obtains mixing A;The step
The speed of agitator of reaction kettle is 240r/min in rapid;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 72 DEG C, vacuum degree is
Reaction 4.5min is mixed under conditions of 0.045MPa, adds tricresyl phosphate (butoxyethyl group) ester and dispersing agent FT- later
Reaction 3.5min is mixed in 78 pressure-maintaining and heat-preservations, obtains mixed material B;The speed of agitator of reaction kettle is 240r/min in the step;
Step 3: taking mixing A and mixed material B to be added in reaction kettle jointly, first temperature is 82 DEG C, vacuum degree is
Reaction 6.5min is mixed under conditions of 0.015MPa, adds illite powder, villus powder and coupling agent later and continues to mix
Conjunction is stirred to react 14min, is eventually adding antioxidant and reaction 4.5min is mixed in crosslinking agent, reaction kettle in the step
Speed of agitator is 320r/min.
Embodiment 3
The present embodiment is related to a kind of fire-retardant high viscous environmental protection type sealing adhesive and preparation method thereof, the sealant by it is following by weight
The raw material of meter forms:
49 parts of vinyl chloride-acrylate copolymer;
35 parts of tertiary butyl phenol aldehyde tackifying resin;
11 parts of 25 μm of partial size of illite powder;
4 parts of methylisothiazolinone;
9 parts of 20 μm of partial size of villus powder;
7 parts of triphenylmethane triisocyanate;
4 parts of flaxseed gum;
5 parts of ester of tricresyl phosphate (butoxyethyl group);
FT-781 parts of dispersing agent;
4 parts of crosslinking agent;
1.3 parts of promotor;
2 parts of antioxidant;
0.5 part of coupling agent.
The selection of crosslinking agent, coupling agent, promotor, antioxidant obtains as shown in table 3 below in above-mentioned raw materials:
Table 3
The preparation method of above-mentioned sealant substantially follows the steps below:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add phase
When the glycerine of the weight of material 10% in reaction kettle, reaction 5min, Zhi Houjia are mixed under conditions of temperature is 60 DEG C
Heat is warming up to 75 DEG C, and triphenylmethane triisocyanate is added and reaction 4min is mixed in promotor, obtains mixing A;The step
The speed of agitator of middle reaction kettle is 250r/min;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 75 DEG C, vacuum degree is
Reaction 4min is mixed under conditions of 0.05MPa, adds tricresyl phosphate (butoxyethyl group) ester later and dispersing agent FT-78 is protected
Reaction 3min is mixed in pressure heat preservation, obtains mixed material B;The speed of agitator of reaction kettle is 250r/min in the step;
Step 3: take mixing A and mixed material B to be added in reaction kettle jointly, first temperature be 85 DEG C, vacuum degree 0.02MPa
Under conditions of be mixed reaction 6min, add illite powder, villus powder and coupling agent later and continues to mix and be stirred to react
12.5min, is eventually adding antioxidant and reaction 4min is mixed in crosslinking agent, and the speed of agitator of reaction kettle is in the step
350r/min。
Embodiment 4
The present embodiment is related to a kind of fire-retardant high viscous environmental protection type sealing adhesive and preparation method thereof, the sealant by it is following by weight
The raw material of meter forms:
50 parts of vinyl chloride-acrylate copolymer;
36 parts of tertiary butyl phenol aldehyde tackifying resin;
12 parts of 30 μm of partial size of illite powder;
4.5 parts of methylisothiazolinone;
10 parts of 30 μm of partial size of villus powder;
7.5 parts of triphenylmethane triisocyanate;
4.5 parts of flaxseed gum;
5.5 parts of ester of tricresyl phosphate (butoxyethyl group);
FT-781.1 parts of dispersing agent;
4.5 parts of crosslinking agent;
1.4 parts of promotor;
2.2 parts of antioxidant;
0.55 part of coupling agent.
The selection of crosslinking agent, coupling agent, promotor, antioxidant obtains as shown in table 4 below in above-mentioned raw materials:
Table 4
The preparation method of above-mentioned sealant substantially follows the steps below:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add phase
When the glycerine of the weight of material 11% in reaction kettle, reaction 4.5min is mixed under conditions of temperature is 62 DEG C, later
78 DEG C are heated to, triphenylmethane triisocyanate is added and reaction 3.5min is mixed in promotor, obtains mixing A;It should
The speed of agitator of reaction kettle is 280r/min in step;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 78 DEG C, vacuum degree is
Reaction 3.5min is mixed under conditions of 0.055MPa, adds tricresyl phosphate (butoxyethyl group) ester and dispersing agent FT- later
Reaction 2.5min is mixed in 78 pressure-maintaining and heat-preservations, obtains mixed material B;The speed of agitator of reaction kettle is 280r/min in the step;
Step 3: taking mixing A and mixed material B to be added in reaction kettle jointly, first temperature is 88 DEG C, vacuum degree is
Reaction 5.5min is mixed under conditions of 0.025MPa, adds illite powder, villus powder and coupling agent later and continues to mix
Conjunction is stirred to react 11min, is eventually adding antioxidant and reaction 3.5min is mixed in crosslinking agent, reaction kettle in the step
Speed of agitator is 380r/min.
Embodiment 5
The present embodiment is related to a kind of fire-retardant high viscous environmental protection type sealing adhesive and preparation method thereof, the sealant by it is following by weight
The raw material of meter forms:
52 parts of vinyl chloride-acrylate copolymer;
40 parts of tertiary butyl phenol aldehyde tackifying resin;
14 parts of 30 μm of partial size of illite powder;
5 parts of methylisothiazolinone;
11 parts of 30 μm of partial size of villus powder;
8 parts of triphenylmethane triisocyanate;
5 parts of flaxseed gum;
6 parts of ester of tricresyl phosphate (butoxyethyl group);
FT-781.2 parts of dispersing agent;
5 parts of crosslinking agent;
1.5 parts of promotor;
2.5 parts of antioxidant;
0.6 part of coupling agent.
The selection of crosslinking agent, coupling agent, promotor, antioxidant obtains as shown in table 5 below in above-mentioned raw materials:
Table 5
The preparation method of above-mentioned sealant substantially follows the steps below:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add phase
When the glycerine of the weight of material 12% in reaction kettle, reaction 4min, Zhi Houjia are mixed under conditions of temperature is 65 DEG C
Heat is warming up to 80 DEG C, and triphenylmethane triisocyanate is added and reaction 3min is mixed in promotor, obtains mixing A;The step
The speed of agitator of middle reaction kettle is 300r/min;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 80 DEG C, vacuum degree is
Reaction 3min is mixed under conditions of 0.06MPa, adds tricresyl phosphate (butoxyethyl group) ester later and dispersing agent FT-78 is protected
Reaction 2min is mixed in pressure heat preservation, obtains mixed material B;The speed of agitator of reaction kettle is 300r/min in the step;
Step 3: take mixing A and mixed material B to be added in reaction kettle jointly, first temperature be 90 DEG C, vacuum degree 0.03MPa
Under conditions of be mixed reaction 5min, add illite powder, villus powder and coupling agent later and continues to mix and be stirred to react
10min, is eventually adding antioxidant and reaction 3min is mixed in crosslinking agent, and the speed of agitator of reaction kettle is in the step
400r/min。
Comparative example 1
This comparative example is related to a kind of sealant, relative to embodiment 1, by vinyl chloride-acrylate copolymer and tertiary butyl phenol
Two kinds of base-materials of aldehyde tackifying resin are exchanged with generating polyurethane resin, other raw materials and content and the preparation method of sealant and embodiment
1 is identical.
Comparative example 2
This comparative example is related to a kind of sealant, relative to embodiment 2, there is only the difference of crosslinker component, other raw materials
And content and the preparation method of sealant it is same as Example 2;
The ingredient of crosslinking agent in this comparative example are as follows: methacrylic acid and hydroxy-ethyl acrylate, mass ratio are also 1:1.
Comparative example 3
This comparative example is related to a kind of sealant, relative to embodiment 3, there is only the difference of coupling agent ingredient, other raw materials
And content and the preparation method of sealant it is same as Example 3;
The ingredient of coupling agent in this comparative example are as follows: gamma-aminopropyl-triethoxy-silane.
Comparative example 4
This comparative example is related to a kind of sealant, relative to embodiment 4, there is only the difference of promotor ingredient, other raw materials
And content and the preparation method of sealant it is same as Example 4;
The ingredient of promotor in this comparative example are as follows: tetramethyl thiourea.
Comparative example 5
This comparative example is related to a kind of sealant, relative to embodiment 5, there is only the difference of antioxidant ingredient, other raw materials
And content and the preparation method of sealant it is same as Example 5;
The ingredient of antioxidant in this comparative example are as follows: antioxidant 1010.
Comparative example 6
This comparative example is related to a kind of sealant, relative to embodiment 5, there is only the difference of preparation method, material composition and
Content is same as Example 5:
The sealant of this comparative example the preparation method is as follows:
It will be added in reaction kettle jointly except other all raw materials of crosslinking agent, temperature is 75 DEG C, vacuum degree is
Reaction 20min is mixed under conditions of 0.06MPa, crosslinking agent, the stirring of present invention kettle is added in 65s before reaction terminates
Revolving speed is 250r/min.
Comparative example 7
This comparative example is related to a kind of commercially available common sealant, which is the raw material for including following parts by weight meter:
70 parts of base polyurethane prepolymer for use as, 30 parts of bisphenol A type epoxy resin, 10 parts of polyisobutene, 5 parts of two amido diphenyl-methane,
5 parts of m-phenylene diamine (MPD), 2 parts of 2-methylimidazole, 2 parts of dibutyl phthalate, 4 parts of calcium carbonate, 2 parts of stearic acid, 8 parts of zinc oxide,
8 parts of aluminium hydroxide, 1.5 parts of Silane coupling agent KH550,1 part of thixotropic agent, TDMD1.5 parts of promotor.
Performance detection
For the beneficial effect for verifying the present invention, such as the following table 6 is carried out to the sealant of above-described embodiment 1-5 and comparative example 1-7
With the detection of 7 performance indicator of table, the sealant of embodiment 1-5, which respectively corresponds, is named as #1-#5, the sealant point of comparative example 1-7
It Dui Ying be named as #6-#12, examination criteria is referring to national standard " GB/T24267-2009 flame retardant sealant for building ": table 6
Table 7
In conjunction with upper table 6 and table 7 it follows that
Compared to national standard: sealant of the invention reduces 53.3-60.0% on surface drying time, on elastic restoration ratio
25.2-72.2% is improved, 187.5-200.0% is improved in tensile strength, improves 84.0- on elongation at break
91.1%;
Compared to comparative example: sealant of the invention reduces 12.5-55.6% on surface drying time, mentions on elastic restoration ratio
High 13.0.2-61.0% improves 43.8-200.0% in tensile strength, improves 19.7-72.0% on elongation at break;
And other physical properties, temperature tolerance, cementability, in terms of on all have and promoted significantly comprehensively,
Progress is obvious compared with prior art, and technical solution does not have apparent property.
In conjunction with beneficial effects of the present invention, applicant carries out the preparation method of part composition and sealant in the present invention
It is following to illustrate:
(1) crosslinking agent: acrylic compounds internal crosslinker is the most common one kind of high molecular material, originally applicant uses it
Single composition or composite components do not obtain desired technical effect, are having been surprisingly found that after many experiments, triallyl isocyanide
The collaboration of two kinds of urea acid esters, polyethyleneglycol diacrylate compositions is used in combination, and can be realized the purpose of the present invention, can make the present invention
Sealant quickly forms bridged bond that is a large amount of and being evenly distributed, the 3 D stereo reticular structure being built into surface drying solidification process
It is form compact and stable, and then improve the strength physical performance of glue-line;If the change of the composition of crosslinking agent or/and content in the present invention,
Will lead to beneficial effects of the present invention cannot realize well.
(2) coupling agent: gamma-aminopropyl-triethoxy-silane is more common a kind of silane in sealant preparation production
It is coupling agent, but is applied in raw materials for production system of the present invention as independent composition, and improper, it is difficult to reaches the present invention
Purpose, subsequent applicant is dexterously by gamma-aminopropyl-triethoxy-silane, rare-earth coupling agent (3-5) in mass ratio: (1-2)
Collaboration utilizes, and unexpectedly obtains corresponding technical effect, physical property, in terms of all have and significantly mention
It rises;If the change of the composition of coupling agent or/and content in the present invention, will lead to beneficial effects of the present invention cannot be good
It realizes.
(3) promotor: applicant is had found by many experiments, using tetramethyl thiourea, accelerant C hartwellB-
515.71W is according to mass ratio (1-2): it is more suitable for that raw material of the invention prepares body that (2-3), which merges obtained mixed type promotor,
System, the coordinated effect of tetramethyl thiourea, accelerant C hartwellB-515.71W can greatly improve reaction and promote efficiency,
It is effectively improved the comprehensive performance of finished product sealant;If the change of the composition of promotor or/and content, will lead in the present invention
Beneficial effects of the present invention cannot be realized well.
(4) antioxidant: likewise, the selection of antioxidant composition of the present invention is not arbitrarily to obtain or there is originally,
It is also what applicant was obtained by many experiments, in development, applicant has been surprisingly found that the collaboration of antioxidant 1010, irgasfos 168
It is used in combination, is more suitable for the preparation reaction system of sealant of the present invention, uses above two composition according to mass ratio (3-
5): (2-3), which merges, to be utilized, and can improve the inoxidizability, stability and service life of glue-line significantly;If resisting in the present invention
The composition of oxygen agent 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 sealant 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 sealant of the present invention, in conjunction with the embodiment of the present invention it can be seen that, system of the invention
Raw material is added using I-III three step design in Preparation Method by several times in batches, and step is simple and orderly, rather than uses the prior art normal
Rule are added at one time (such as comparative example 6), and this technique is the special proportion phase with sealant raw materials for production component of the present invention
It adapts to, only uses this technique, just can guarantee the excellent characteristics for the sealant finally prepared.
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 fire-retardant high viscous environmental protection type sealing adhesive, which is characterized in that be made of following raw material by weight:
52 parts of vinyl chloride-acrylate copolymer;
40 parts of tertiary butyl phenol aldehyde tackifying resin;
14 parts of 30 μm of partial size of illite powder;
5 parts of methylisothiazolinone;
11 parts of 30 μm of partial size of villus powder;
8 parts of triphenylmethane triisocyanate;
5 parts of flaxseed gum;
6 parts of ester of tricresyl phosphate (butoxyethyl group);
1.2 parts of dispersing agent FT-78;
5 parts of crosslinking agent;
1.5 parts of promotor;
2.5 parts of antioxidant;
0.6 part of coupling agent.
2. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 1, which is characterized in that the preparation side of the sealant
Method is as follows:
Step 1: taking vinyl chloride-acrylate copolymer, tertiary butyl phenol aldehyde tackifying resin to be added in reaction kettle, add and be equivalent to
Reaction 4min is mixed in the glycerine of weight of material 12% in reaction kettle under conditions of temperature is 65 DEG C, and heating rises later
Temperature is added triphenylmethane triisocyanate and reaction 3min is mixed in promotor, obtain mixing A to 80 DEG C;
Step 2: taking flaxseed gum, methylisothiazolinone to be added in reaction kettle, temperature is 80 DEG C, vacuum degree is
Reaction 3min is mixed under conditions of 0.06MPa, adds tricresyl phosphate (butoxyethyl group) ester later and dispersing agent FT-78 is protected
Reaction 2min is mixed in pressure heat preservation, obtains mixed material B;
Step 3: taking mixing A and mixed material B to be added in reaction kettle jointly, first in the item that temperature is 90 DEG C, vacuum degree is 0.03MPa
Reaction 5min is mixed under part, adds illite powder, villus powder and coupling agent later and continuess to mix and be stirred to react
10min, is eventually adding antioxidant and reaction 3min is mixed in crosslinking agent.
3. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 2, which is characterized in that the stirring of the reaction kettle turns
Speed is 300-400r/min.
4. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 1, which is characterized in that the crosslinking agent is three allyls
Two kinds of base isocyanuric acid ester, polyethyleneglycol diacrylate compositions merge.
5. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 4, which is characterized in that the crosslinking agent is three allyls
Base isocyanuric acid ester, polyethyleneglycol diacrylate merge according to mass ratio 2:3.
6. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 1, which is characterized in that the coupling agent is γ-ammonia
Two kinds of propyl-triethoxysilicane, rare-earth coupling agent compositions merge.
7. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 6, which is characterized in that the coupling agent is γ-ammonia
Propyl-triethoxysilicane, rare-earth coupling agent merge according to mass ratio 5:2.
8. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 1, which is characterized in that the promotor is tetramethyl
Thiocarbamide, accelerant C hartwell B-515.71W merge according to mass ratio 2:3.
9. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 1, which is characterized in that the antioxidant is antioxidant
1010, irgasfos 168 is according to mass ratio (3-5): what (2-3) merging obtained.
10. the fire-retardant high viscous environmental protection type sealing adhesive of one kind according to claim 9, which is characterized in that the antioxidant is antioxygen
Agent 1010, irgasfos 168 merge according to mass ratio 5:3.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111484815A (en) * | 2019-01-25 | 2020-08-04 | 肇庆市联力化工有限公司 | Tackifier for improving adhesive property between rubber and cord |
-
2018
- 2018-07-03 CN CN201810717789.0A patent/CN109021872A/en not_active Withdrawn
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CN111484815A (en) * | 2019-01-25 | 2020-08-04 | 肇庆市联力化工有限公司 | Tackifier for improving adhesive property between rubber and cord |
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