CN108048025A - A kind of single-component mist-solidifying polyurethane sealant and preparation method thereof - Google Patents
A kind of single-component mist-solidifying polyurethane sealant and preparation method thereof Download PDFInfo
- Publication number
- CN108048025A CN108048025A CN201711433156.9A CN201711433156A CN108048025A CN 108048025 A CN108048025 A CN 108048025A CN 201711433156 A CN201711433156 A CN 201711433156A CN 108048025 A CN108048025 A CN 108048025A
- Authority
- CN
- China
- Prior art keywords
- parts
- agent
- acid
- solidifying
- component mist
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
-
- 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
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of single-component mist-solidifying polyurethane sealants, are related to polyurethane sealant technical field, and single-component mist-solidifying polyurethane sealant includes following components：The pure PO polyether polyurethane prepolymers of 100 parts of NCO sealing ends, 40~60 parts of NCO block polyether polyurethane prepolymer containing EO, the unsaturated polyether polyol polyurethane prepolymer of 1~100 part of NCO sealing end, 110~150 parts of plasticizer, 1~2 part of silane coupling agent, 1~2.5 part of deicer, 1.5~3 parts of crosslinking agents, 150~400 parts of inorganic fillers, 30~60 parts of surface matt modifying agent, 0.2~0.4 part of organic acid catalyst, 0.05~0.4 part of organotin catalysts, 0.5~6 part of thixotropic agent, 5~20 parts of latent curing agents.The present invention makes fluid sealant possess free radical polymerization function, can significantly promote its adhesive effect by introducing unsaturated polyether polyol prepolymer into PU body prepolymer.The invention also discloses a kind of preparation methods of single-component mist-solidifying polyurethane sealant.
Description
Technical field
The present invention relates to polyurethane sealant technical fields, and in particular to a kind of single-component mist-solidifying polyurethane seal
Glue and preparation method thereof.
Background technology
Car and large commercial car roof are spliced by plurality of steel plates at present, and technique is generally spot welding spelling
It connects, crosses point swimming, local putty (poly-putty base) is levelling, and then welding position is sealed using fluid sealant rapidly.Fluid sealant
Bonding and sealing surface actually there are two types of, one kind is electrophoresis lacquer painting, and another kind is putty face.This requires fluid sealant first must
Must there will be good adhesive property against two kinds of Facing materials, in addition also to require that gas cannot be generated in the curing process
Bubble, no person may cause large area bulge, influence roof appearance.
Conventional single-component mist-solidifying polyurethane sealant is bonded preferably electrophoresis lacquer painting, but putty plate is glued
Connect poor effect, when peel test is substantially interfacial failure form.Firm sealing can not be formed.This is because putty is
Solidfied material, the composite material that mica powder is main stuffing, the surface polarity of cured product based on unsaturated polyester (UP), styrene
Weaker, in addition the mica powder of lamellar structure reduces further the bonding firmness of material surface, to the bonding of fluid sealant
It is very unfavorable.
In addition conventional single-component mist-solidifying polyurethane sealant in the curing process can carbon dioxide gas,
Aggregation bubble is easy in so cured glue-line, when serious (as in the case of summer high temperature high humidity) if be present with it is serious
Bulge phenomenon, influence the appearance in adhering and sealing face, also entail dangers to sealing effect when serious.
In addition, existing conventional moisture cures polyurethane sealant in use, also there is smeared with liquor of washing one's hands
What the dumb light (glossiness) after usually flowing the problem of Heisui River influences vehicle appearance and storing for a long time after sealing glue solidifying was deteriorated
Problem, it is impossible to meet requirement of the client to appearance.
Therefore, adhesive effect of the conventional single-component mist-solidifying polyurethane sealant on putty face is promoted, is solved simultaneously
The bulge problem of its solidification process can make single-component mist-solidifying polyurethane sealant meet current car and large commercial
The requirement of appearance is a technical problem to be solved urgently after the sealing technology requirement of car roof and client cure product.
The content of the invention
For defect in the prior art, it is an object of the invention to provide a kind of poly- ammonia of single-component mist-solidifying
Ester fluid sealant and preparation method thereof significantly promotes its adhesive effect, and fundamentally alleviates or prevented bubble or bubbling
Problem.
To achieve the above objectives, the present invention adopts the technical scheme that：A kind of single-component mist-solidifying polyurethane seal
Glue, in parts by mass, the single-component mist-solidifying polyurethane sealant include following components：
The pure PO polyether polyurethane prepolymers of 100 parts of NCO sealing ends, 40~60 parts of NCO block the pre-polymerization of polyether-polyurethane containing EO
Object, the unsaturated polyether polyol polyurethane prepolymer of 1~100 part of NCO sealing end, 110~150 parts of plasticizer, 1~2 part of silane
Coupling agent, 1~2.5 part of deicer, 1.5~3 parts of crosslinking agents, 150~400 parts of inorganic fillers, 30~60 parts of surface matts are modified
Agent, 0.2~0.4 part of organic acid catalyst, 0.05~0.4 part of organotin catalysts, 0.5~6 part of thixotropic agent, 5~20 parts it is latent solid
Agent.
Based on the above technical solutions, the pure PO polyether polyurethane prepolymers of the NCO sealing ends are by excessive isocyanide
Acid esters is made with pure PO polyether polyol, catalyst, reaction suppressor reaction, and NCO content is between 2.0~3.0%.
Based on the above technical solutions, the unsaturated polyether polyol polyurethane prepolymer of the NCO sealing ends is by mistake
The isocyanates of amount is made with the polyether polyol containing unsaturated double-bond, catalyst, reaction suppressor reaction, and NCO content exists
Between 2.0~3.0%.
Based on the above technical solutions, the polyether polyurethane prepolymer containing EO of the NCO sealing ends is by excessive isocyanide
Acid esters is made with polyether polyol containing EO, catalyst, reaction suppressor reaction, and NCO content is between 2.0~3.0%.
Based on the above technical solutions, the plasticizer for phenyl alkylsulf, diisononyl phthalate,
One or more in diisooctyl phthalate, polyadipate second binary alcohol esters, polypropylene glycol adipate.
Based on the above technical solutions, the silane coupling agent is amino coupling agent, sulfydryl coupling agent, epoxy group
One or more in coupling agent.
Based on the above technical solutions, the deicer is tolysulfonyl isocyanates, 3- butyl -2- (1- second
One or more in base amyl) oxazolidines, 2- isopropyl -3- oxazolidine ethyl alcohol.
Based on the above technical solutions, the crosslinking agent is the isocyanates of three or more degrees of functionality.
Based on the above technical solutions, the inorganic filler is less than 500ppm for non-surface treated and water content
Inorganic powder, type of powder is kaolin, powdered whiting, talcum powder, carbon black, the one or more in silicon powder.
Based on the above technical solutions, it is micro- that the surface matt modifying agent is talcum powder, PVC pastes resin, polyethylene
One or more in powder.
Based on the above technical solutions, the organic acid catalyst is aliphatic unitary, binary, polybasic carboxylic acid
Or aromatic carboxylic acid, it is maleic acid, fumaric acid, oxalic acid, salicylic acid, tartaric acid, malic acid, citric acid, Vitamin C
One or more in acid, acrylic acid, methacrylic acid, benzoic acid, caffeic acid.
Based on the above technical solutions, the latent curing agent is aldimine or Polyaldimines latent curing agent.
Based on the above technical solutions, the thixotropic agent is hydrophobic fumed silica, polyureas thixotropic agent, poly- third
One or more in acrylamide.
The invention also discloses a kind of a kind of preparation method of single-component mist-solidifying polyurethane sealant, bags
Include following steps：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, adds in what 100 parts of NCO were blocked into glue container
Pure PO polyether polyurethane prepolymers, 40~60 parts of NCO sealing ends polyether polyurethane prepolymers containing EO, 1~100 part of NCO sealing end are not
Saturation polyether polyol polyurethane prepolymer, 110~150 parts of plasticizer, 1~2 part of silane coupling agent, 1~2.5 part of deicer,
It is stirred below uniform to material to be evacuated to -0.098Mpa for 1.5~3 parts of crosslinking agents；
Nitrogen protects pressure release, adds in 150~400 parts of inorganic fillers and 30~60 parts of surface matt modifying agent, vacuumizes
To below -0.098Mpa, simultaneously 20~35 DEG C of stirrings of temperature control are uniform to material；
Nitrogen protection pressure release, 0.2~0.4 part of organic acid catalyst of addition, 0.05~0.4 part of organotin catalysts, 0.5
~6 parts of thixotropic agent, 5~20 parts of latent curing agents, are evacuated to below -0.098Mpa and 20~35 DEG C of stirrings of temperature control are equal to material
It is even.
Compared with prior art, the advantage of the invention is that：
The present invention is by introducing unsaturated segment (unsaturated polyether polyol pre-polymerization into PU body prepolymer
Object), fluid sealant is made to possess free radical polymerization function.Since the time very short after roof Puttying begins to apply fluid sealant, gluing
When putty be not yet fully cured, therefore after fluid sealant is coated onto on putty plate, in fluid sealant with the unsaturated chain of putty contact portion
Section prepolymer can be participated in the curing cross-linking process of putty, can significantly promote its adhesive effect.
In addition present invention introduces part latent curing agent, further to conventional single-component mist-solidifying polyurethane sealant
Curing mode is improved, and more thoroughly solves the problems, such as its bubble and bubbling.Under conditions of having latent curing agent, moisture and
Latent curing agent reaction releases polyamine (binary and more than) and the macromolecular aldehyde of liquid, and polyamine carries out instead rapidly with-NCO
Crosslinking should be generated, the liquid macromolecular aldehyde of this process release is not related to the release of carbon dioxide, therefore fundamentally delays
It solves or has prevented bubble or the problem of bubbling.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
The embodiment of the present invention provides a kind of single-component mist-solidifying polyurethane sealant, in parts by mass, one-pack moisture
Curing polyurethane sealant includes following components：
The pure PO polyether polyurethane prepolymers of 100 parts of NCO sealing ends, 40~60 parts of NCO block the pre-polymerization of polyether-polyurethane containing EO
Object, the unsaturated polyether polyol polyurethane prepolymer of 1~100 part of NCO sealing end, 110~150 parts of plasticizer, 1~2 part of silane
Coupling agent, 1~2.5 part of deicer, 1.5~3 parts of crosslinking agents, 150~400 parts of inorganic fillers, 30~60 parts of surface matts are modified
Agent, 0.2~0.4 part of organic acid catalyst, 0.05~0.4 part of organotin catalysts, 0.5~6 part of thixotropic agent, 5~20 parts it is latent solid
Agent.
The pure PO polyether polyurethane prepolymers of NCO sealing ends are by excessive isocyanates and pure PO polyether polyol, catalysis
Agent, reaction suppressor reaction are made, it is preferred that its NCO content is between 2.0~3.0%.
The unsaturated polyether polyol polyurethane prepolymer of NCO sealing ends is by excessive isocyanates with containing unsaturated double-bond
Polyether polyol, catalyst, reaction suppressor reaction be made, it is preferred that its NCO content is between 2.0~3.0%.
The polyether polyurethane prepolymer containing EO of NCO sealing ends is by excessive isocyanates and polyether polyol containing EO, catalysis
Agent, reaction suppressor reaction are made, it is preferred that its NCO content is between 2.0~3.0%.
Plasticizer is phenyl alkylsulf, diisononyl phthalate, diisooctyl phthalate, polyadipate
One or more in second binary alcohol esters, polypropylene glycol adipate.
Silane coupling agent is the one or more in amino coupling agent, sulfydryl coupling agent, epoxy group coupling agent.
Deicer is tolysulfonyl isocyanates, 3- butyl -2- (1- ethyl pentyl group) oxazolidines, 2- isopropyl -3- Evil
One or more in oxazolidine ethyl alcohol.
Crosslinking agent is the isocyanates of three or more degrees of functionality.
Inorganic filler is less than the inorganic powder of 500ppm, the preferred kaolinite of type of powder for non-surface treated and water content
One or more in soil, powdered whiting, talcum powder, carbon black, silicon powder.
Surface matt modifying agent is talcum powder, the one or more in PVC paste resin, polyethylene micropowder.
Organic acid catalyst be aliphatic unitary, binary, polybasic carboxylic acid or aromatic carboxylic acid, preferably maleic acid,
Fumaric acid, oxalic acid, salicylic acid, tartaric acid, malic acid, citric acid, ascorbic acid, acrylic acid, methacrylic acid, benzene first
One or more in acid, caffeic acid.
Latent curing agent is aldimine or Polyaldimines latent curing agent.
Thixotropic agent is hydrophobic fumed silica, the one or more in polyureas thixotropic agent, polyacrylamide.
Pure PO polyether polyurethane prepolymers, the unsaturated polyether polyol polyurethane prepolymer of NCO sealing ends of NCO sealing ends
Or the preparation method of the polyether polyurethane prepolymer containing EO of NCO sealing ends, comprise the following steps：
In terms of mass parts, by pure PO, unsaturated polyether polyol or polyether polyol containing EO at 120 DEG C and less than-
0.098Mpa vacuum under pressure is dehydrated to bubble-free, is cooled to less than 50 DEG C, is put into isocyanates by metered proportions, is mixed
Add in catalyst after closing uniformly, the protection of dry nitrogen, the reaction of 65~80 DEG C of temperature control, every 30min sampling and testing NCO contents,
When NCO content reaches design proportion and keeps stablizing, reaction suppressor is added in, continues to stir 30min, cooling discharge.
The embodiment of the invention also discloses a kind of preparation method of single-component mist-solidifying polyurethane sealant, including with
Lower step：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, adds in what 100 parts of NCO were blocked into glue container
Pure PO polyether polyurethane prepolymers, 40~60 parts of NCO sealing ends polyether polyurethane prepolymers containing EO, 1~100 part of NCO sealing end are not
Saturation polyether polyol polyurethane prepolymer, 110~150 parts of plasticizer, 1~2 part of silane coupling agent, 1~2.5 part of deicer,
It is stirred below uniform to material to be evacuated to -0.098Mpa for 1.5~3 parts of crosslinking agents；
Nitrogen protects pressure release, adds in 150~400 parts of inorganic fillers and 30~60 parts of surface matt modifying agent, vacuumizes
To below -0.098Mpa, simultaneously 20~35 DEG C of stirrings of temperature control are uniform to material；
Nitrogen protection pressure release, 0.2~0.4 part of organic acid catalyst of addition, 0.05~0.4 part of organotin catalysts, 0.5
~6 parts of thixotropic agent, 5~20 parts of latent curing agents, are evacuated to below -0.098Mpa and 20~35 DEG C of stirrings of temperature control are equal to material
It is even.
Embodiment 1：
Single-component mist-solidifying polyurethane sealant provided in this embodiment, including
Prepolymer synthesizes：
The synthesis of the pure PO polyether polyurethane prepolymers (PP-1) of NCO sealing ends：
Pure PO polyethers WT-5000 (manufacturer's DOW Chemical, three-functionality-degree, average molecular weight 5000) 4250g is taken to add in four
Mouth flask, is heated to 120 DEG C, vacuumizes dehydration, below vacuum pressure -0.098Mpa, until bubble-free is emerged, stops dehydration；
Cooling down adds in 750gMDI to less than 80 DEG C, and nitrogen protection stirring to MDI is completely dissolved.Temperature is controlled 50~60
DEG C, 0.02g dibutyl tin laurates are added in, 70 DEG C of reaction 2h of temperature control, it is 2.85% to survey NCO contents.Discharging, nitrogen charging are airtight
Envelope preserves for use.
The synthesis of NCO sealing end polyether polyurethane prepolymers containing EO (PE-1)：
The poly- 330N of polyethers containing EO (manufacturer Shandong east is big, three-functionality-degree, average molecular weight 5000) 4250g is taken to add in four
Mouth flask, is heated to 120 DEG C, vacuumizes dehydration, below vacuum pressure -0.098Mpa, until bubble-free is emerged, stops dehydration；
Cooling down adds in 750gMDI to less than 80 DEG C, and nitrogen protection stirring to MDI is completely dissolved.Temperature is controlled at 50~60 DEG C,
0.02g dibutyl tin laurates are added in, 70 DEG C of reaction 2h of temperature control, it is 2.83% to survey NCO content.Discharging, nitrogen charging hermetic seal are protected
It deposits for use.
The synthesis of the unsaturated polyether polyol polyurethane prepolymer (PI-1) of NCO sealing ends：
Take unsaturated polyether polyol PloybdR45V (manufacturer's Cray Willie, 2.4 degrees of functionality, average molecular weight
2800) 4134g adds in four-hole boiling flask, adds in 2g tosyls isocyanates (PTSI), nitrogen protection stirring 15min；It is follow-up
It is continuous to add in 866gMDI, 50~60 DEG C are warming up to, nitrogen protection stirring to MDI is completely dissolved.Temperature is maintained at 50~60 DEG C,
0.02g dibutyl tin laurates are added in, 70 DEG C of reaction 2h of temperature control, it is 2.85% to survey NCO content.Discharging, nitrogen charging hermetic seal are protected
It deposits for use.
Fluid sealant 1 is formulated：
100 parts of above-mentioned PP-1,40 parts of PE-1,1 part of PI-1,110 parts of phenyl alkylsulfs Mesamoll, 1 part of coupling agent A-
171,1 parts of deicer PTSI, 1.5 parts of HDI trimers, 150 parts of calcined kaolins, 5 parts of carbon blacks, 30 parts of PVC paste resins, 0.5 part
Aerosil, 0.2 part of maleic acid, 0.05 part of dibutyl tin laurate, 5 parts of IncozolBH latent curing agents.
Note：Phenyl alkylsulf Mesamoll, manufacturer Lang Sheng；Deicer PTSI, also referred to as tolysulfonyl isocyanic acid
Ester, German OMGBorchers；HDI trimer, also referred to as hexamethylene diisocyanate trimer, German Baeyer；PVC paste tree
Fat, Sol dimension；IncozolBH latent curing agents, Britain Incozol.
A kind of preparation process of above-mentioned single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and 100 parts of above-mentioned PP-1 are added in into glue container,
40 parts of PE-1,1 part of PI-1,110 parts of phenyl alkylsulf Mesamoll, 1 part of coupling agent A-171,1 part of deicer PTSI, 1.5
Part HDI trimer, it is stirred below uniform to material to be evacuated to -0.098Mpa；After reaching requirement, nitrogen protection pressure release, quickly
150 parts of calcined kaolins of addition, 5 parts of carbon blacks, 30 parts of PVC paste resins, 0.5 part of aerosil, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa；After reaching requirement, nitrogen protection pressure release is quick to add
Enter 0.2 part of maleic acid, 0.05 part of dibutyl tin laurate, 5 parts of IncozolBH latent curing agents, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa, and discharging packing is for use after reaching requirement.
Embodiment 2：
Single-component mist-solidifying polyurethane sealant provided in this embodiment, including
Prepolymer synthesizes：
The synthesis of the pure PO polyether polyurethane prepolymers (PP-2) of NCO sealing ends：
Take pure PO polyethers VORANOL230-042N (manufacturer's DOW Chemical, three-functionality-degree, average molecular weight 4000)
4218g adds in four-hole boiling flask, is heated to 120 DEG C, vacuumizes dehydration, below vacuum pressure -0.098Mpa, until bubble-free emits
Go out, stop dehydration；Cooling down adds in 782gMDI to less than 80 DEG C, and nitrogen protection stirring to MDI is completely dissolved.Control temperature
Degree adds in 0.02g dibutyl tin laurates, 70 DEG C of reaction 2h of temperature control, it is 2.60% to survey NCO content at 50~60 DEG C.Go out
Material, inflated with nitrogen are sealed for use.
The synthesis of NCO sealing end polyether polyurethane prepolymers containing EO (PE-2)：
Take the poly- VORANOLCP6055 of polyethers containing EO (manufacturer's DOW Chemical, three-functionality-degree, average molecular weight 6000)
4342g adds in four-hole boiling flask, is heated to 120 DEG C, vacuumizes dehydration, below vacuum pressure -0.098Mpa, until bubble-free emits
Go out, stop dehydration；Cooling down adds in 658gMDI to less than 80 DEG C, and nitrogen protection stirring to MDI is completely dissolved.Control temperature
Degree adds in 0.02g dibutyl tin laurates, 70 DEG C of reaction 2h of temperature control, it is 2.59% to survey NCO content at 50~60 DEG C.Go out
Material, inflated with nitrogen are sealed for use.
The synthesis of the unsaturated polyether polyol polyurethane prepolymer (PI-2) of NCO sealing ends：
Take unsaturated polyether polyol PloybdR20LM (manufacturer's Cray Willie, 2.4 degrees of functionality, average molecular weight
1200) 3691g adds in four-hole boiling flask, adds in 2g tosyls isocyanates (PTSI), nitrogen protection stirring 15min；It is follow-up
It is continuous to add in 1309gMDI, 50~60 DEG C are warming up to, nitrogen protection stirring to MDI is completely dissolved.Temperature is maintained at 50~60 DEG C,
0.02g dibutyl tin laurates are added in, 70 DEG C of reaction 2h of temperature control, it is 2.60% to survey NCO content.Discharging, nitrogen charging hermetic seal are protected
It deposits for use.
Fluid sealant 2 is formulated：
100 parts of above-mentioned PP-2,50 parts of PE-2,10 parts of PI-2,130 parts of phenyl alkylsulf Mesamoll, 1.5 parts of couplings
Agent A-171,2.5 parts of deicer PTSI, 2 parts of HDI trimers, 200 parts of powdered whitings, 5 parts of carbon blacks, 50 parts of PVC paste resins, 2
Part aerosil, 0.4 part of maleic acid, 0.1 part of dibutyl tin laurate, 12 parts of IncozolBH latent curing agents.
A kind of preparation process of above-mentioned single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and 100 parts of above-mentioned PP-2 are added in into glue container,
50 parts of PE-2,10 parts of PI-2,130 parts of phenyl alkylsulf Mesamoll, 1.5 parts of coupling agent A-171,2.5 parts of deicers
It is stirred below uniform to material to be evacuated to -0.098Mpa for PTSI, 2.0 parts of HDI trimers；After reaching requirement, nitrogen protection
Pressure release, rapidly joins 200 parts of powdered whitings, 5 parts of carbon blacks, 50 parts of PVC paste resins, 2 parts of aerosils, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa；After reaching requirement, nitrogen protection pressure release is quick to add
Enter 0.4 part of maleic acid, 0.1 part of dibutyl tin laurate, 7 parts of IncozolBH latent curing agents, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa, and discharging packing is for use after reaching requirement.
Embodiment 3：
Single-component mist-solidifying polyurethane sealant provided in this embodiment, including
The synthesis of the unsaturated polyether polyol polyurethane prepolymer (PI-3) of NCO sealing ends：
Take unsaturated polyether polyol KrasolLBH (P) 2000 (manufacturer's Cray Willie, 1.9 degrees of functionality, mean molecule
2000) 4123g adds in four-hole boiling flask to amount, adds in 2g tosyls isocyanates (PTSI), nitrogen protection stirring 15min；Afterwards
877gMDI is continuously added, is warming up to 50~60 DEG C, nitrogen protection stirring to MDI is completely dissolved.Temperature is maintained at 50~60 DEG C,
0.02g dibutyl tin laurates are added in, 70 DEG C of reaction 2h of temperature control, it is 2.60% to survey NCO content.Discharging, nitrogen charging hermetic seal are protected
It deposits for use.
Fluid sealant 3 is formulated：
100 parts of above-mentioned PP-2,60 parts of PE-2,100 parts of PI-3,120 parts of phenyl alkylsulf Mesamoll, 1.5 parts of couplings
Agent A-171,2.0 parts of deicer PTSI, 2 parts of HDI trimers, 200 parts of calcined kaolins, 20 parts of carbon blacks, 60 parts of PVC paste resins,
6 parts of aerosils, 0.4 part of maleic acid, 0.2 part of dibutyl tin laurate, 20 parts of IncozolBH dive curing
Agent.
A kind of preparation process of above-mentioned single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and 100 parts of above-mentioned PP-2 are added in into glue container,
60 parts of PE-2,100 parts of PI-3,120 parts of phenyl alkylsulf Mesamoll, 1.5 parts of coupling agent A-171,2.0 parts of deicers
It is stirred below uniform to material to be evacuated to -0.098Mpa for PTSI, 2 parts of HDI trimers；After reaching requirement, nitrogen protection is let out
Pressure, quick plus 200 parts of calcined kaolins, 20 parts of carbon blacks, 60 parts of PVC paste resins, 6 parts of aerosils, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa；After reaching requirement, nitrogen protection pressure release is quick to add
Enter 0.4 part of maleic acid, 0.2 part of dibutyl tin laurate, 20 parts of IncozolBH latent curing agents, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa, and discharging packing is for use after reaching requirement.
Embodiment 4：
Fluid sealant 4 is formulated：
100 parts of above-mentioned PP-1,40 parts of PE-1,80 parts of PI-1,110 parts of phenyl alkylsulf Mesamoll, 1 part of coupling agent
A-171,1 part of deicer PTSI, 1.5 parts of HDI trimers, 380 parts of calcined kaolins, 20 parts of carbon blacks, 50 parts of PVC paste resins, 3
Part aerosil, 0.3 part of maleic acid, 0.1 part of dibutyl tin laurate, 15 parts of IncozolBH latent curing agents.
A kind of preparation process of above-mentioned single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and 100 parts of above-mentioned PP-1 are added in into glue container,
40 parts of PE-1,80 parts of PI-1,110 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI, 1.5 parts of HDI trimers, pumping is very
It is empty stirred below uniform to material to -0.098Mpa；After reaching requirement, it is high to rapidly join 380 parts of calcinings for nitrogen protection pressure release
Ridge soil, 20 parts of carbon blacks, 50 parts of PVC paste resins, 3 parts of aerosils, be evacuated to below -0.098Mpa and temperature control 20~
35 DEG C of high-speed stirreds are uniform to material；After reaching requirement, nitrogen protection pressure release rapidly joins 0.3 part of maleic acid, 0.1 part
Dibutyl tin laurate, 15 parts of IncozolBH latent curing agents are evacuated to below -0.098Mpa simultaneously 20~35 DEG C of temperature control
High-speed stirred is uniform to material, and discharging packing is for use after reaching requirement.
Embodiment 5：
Fluid sealant 5 is formulated：
100 parts of above-mentioned PP-1,50 parts of PE-1,100 parts of PI-1,75 parts of DIDP, 75 parts of phenyl alkylsulf Mesamoll, 1
Part coupling agent A-171,1 part of deicer PTSI, 1.5 parts of HDI trimers, 250 parts of powdered whitings, 100 parts of carbon blacks, 50 parts of PVC
Paste resin, 0.5 part of aerosil, 0.3 part of maleic acid, 0.1 part of dibutyl tin laurate, 15 parts
IncozolBH latent curing agents.
A kind of preparation process of above-mentioned single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, 100 parts of above-mentioned PP-1 of addition into glue container, and 50
Part PE-1,100 parts of PI-1,75 parts of DIDP, 75 parts of phenyl alkylsulf Mesamoll, 1 part of coupling agent A-171,1 part of deicer
It is stirred below uniform to material to be evacuated to -0.098Mpa for PTSI, 1.5 parts of HDI tripolymers；After reaching requirement, nitrogen protection
Pressure release rapidly joins 250 parts of powdered whitings, 100 parts of carbon blacks, and 50 parts of PVC paste resin, and 0.5 part of aerosil is taken out true
It is empty that below -0.098Mpa, simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material；After reaching requirement, nitrogen protection pressure release, soon
Speed 0.3 part of maleic acid of addition, 0.1 part of dibutyl tin laurate, 15 parts of IncozolBH latent curing agents, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa, and discharging packing is for use after reaching requirement.
Comparative example 1：
A kind of existing single-component mist-solidifying polyurethane sealant, including
Fluid sealant 6 is formulated：
100 parts of PE-1,100 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI, 100 parts of calcined kaolins, 30
Part carbon black, 50 parts of PVC paste resins, 1 part of aerosil, 0.2 part of dibutyl tin laurate.
The preparation process of above-mentioned existing single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, 100 parts of PE-1 of addition into glue container, 100 parts
It is stirred below uniform to material to be evacuated to -0.098Mpa by DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI；Reaching will
After asking, nitrogen protection pressure release rapidly joins 100 parts of calcined kaolins, 30 parts of carbon blacks, 50 parts of PVC paste resins, 1 part of gas phase two
Silica, is evacuated to below -0.098Mpa and 20~35 DEG C of high-speed stirreds of temperature control are uniform to material；After reaching requirement, nitrogen
Pressure release is protected, rapidly joins 0.2 part of dibutyl tin laurate, is evacuated to below -0.098Mpa simultaneously 20~35 DEG C of height of temperature control
Speed stirring is uniform to material, and discharging packing is for use after reaching requirement.
Comparative example 2：
A kind of existing single-component mist-solidifying polyurethane sealant, including
Fluid sealant 7 is formulated：
100 parts of PP-1,100 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI, 100 parts of calcined kaolins, 50
Part carbon black, 50 parts of PVC paste resins, 1 part of aerosil, 0.2 part of dibutyl tin laurate.
The preparation process of above-mentioned existing single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, 100 parts of PP-1 of addition into glue container, 100 parts
It is stirred below uniform to material to be evacuated to -0.098Mpa by DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI；Reaching will
After asking, nitrogen protection pressure release rapidly joins 100 parts of calcined kaolins, 50 parts of carbon blacks, 50 parts of PVC paste resins, 1 part of gas phase two
Silica, is evacuated to below -0.098Mpa and 20~35 DEG C of high-speed stirreds of temperature control are uniform to material；After reaching requirement, nitrogen
Pressure release is protected, rapidly joins 0.2 part of dibutyl tin laurate, is evacuated to below -0.098Mpa simultaneously 20~35 DEG C of height of temperature control
Speed stirring is uniform to material, and discharging packing is for use after reaching requirement.
Comparative example 3：
A kind of existing single-component mist-solidifying polyurethane sealant, including
Fluid sealant 8 is formulated：
100 parts of PP-1,50 parts of PE-1,120 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI, 150 parts are calcined
Kaolin, 50 parts of carbon blacks, 50 parts of PVC paste resins, 1 part of aerosil, 0.2 part of dibutyl tin laurate.
The preparation process of above-mentioned existing single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, 100 parts of PP-1 of addition into glue container, 50 parts
It is stirred below to material to be evacuated to -0.098Mpa by PE-1,120 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI
Uniformly；After reaching requirement, nitrogen protection pressure release rapidly joins 150 parts of calcined kaolins, 50 parts of PVC paste resins, 1 part of gas phase
Silica, is evacuated to below -0.098Mpa and 20~35 DEG C of high-speed stirreds of temperature control are uniform to material；After reaching requirement, nitrogen
Gas shielded pressure release rapidly joins 0.2 part of dibutyl tin laurate, is evacuated to below -0.098Mpa simultaneously 20~35 DEG C of temperature control
High-speed stirred is uniform to material, and discharging packing is for use after reaching requirement.
Comparative example 4：
A kind of existing single-component mist-solidifying polyurethane sealant, including
Fluid sealant 9 is formulated：
100 parts of above-mentioned PP-1,50 parts of PE-1,150 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI, 250 parts
Powdered whiting, 100 parts of carbon blacks, 50 parts of PVC paste resins, 0.5 part of aerosil, 0.1 part of dibutyl tin laurate.
The preparation process of above-mentioned existing single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and 100 parts above-mentioned 100 parts are added in into glue container
Above-mentioned PP-1,50 parts of PE-1,150 parts of DIDP, 1 part of coupling agent A-171,1 part of deicer PTSI, be evacuated to -0.098Mpa with
Lower stirring is uniform to material；After reaching requirement, nitrogen protection pressure release rapidly joins 250 parts of powdered whitings, 100 parts of carbon blacks,
50 parts of PVC paste resins, 0.5 part of aerosil are evacuated to below -0.098Mpa simultaneously 20~35 DEG C of high-speed stirreds of temperature control
It is uniform to material；After reaching requirement, nitrogen protection pressure release rapidly joins 0.1 part of dibutyl tin laurate, be evacuated to-
Simultaneously 20~35 DEG C of high-speed stirreds of temperature control are uniform to material by below 0.098Mpa, and discharging packing is for use after reaching requirement.
Comparative example 5
Fluid sealant 10 is formulated：
100 parts of above-mentioned PP-1,50 parts of PE-1,100 parts of PI-1,150 parts of DINP, 1 part of coupling agent A-171,1 part of deicer
PTSI, 1.5 parts of HDI trimers, 250 parts of powdered whitings, 100 parts of carbon blacks, 50 parts of PVC paste resins, 0.5 part of gas phase titanium dioxide
Silicon, 0.3 part of maleic acid, 0.1 part of dibutyl tin laurate, 15 parts of IncozolBH latent curing agents.
A kind of preparation process of above-mentioned single-component mist-solidifying polyurethane sealant is as follows：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and 100 parts of above-mentioned PP-1 are added in into glue container,
40 parts of PE-1,80 parts of PI-1,150 parts of DINP, 1 part of coupling agent A-171,1 part of deicer PTSI, 1.5 parts of HDI trimers, pumping is very
It is empty stirred below uniform to material to -0.098Mpa；After reaching requirement, it is high to rapidly join 400 parts of calcinings for nitrogen protection pressure release
Ridge soil, 50 parts of PVC paste resins, 3 parts of aerosils are evacuated to below -0.098Mpa simultaneously 20~35 DEG C of high-speed stirrings of temperature control
It mixes uniform to material；After reaching requirement, nitrogen protection pressure release rapidly joins 0.3 part of maleic acid, 0.1 part of tin dilaurate two
Butyl tin, 15 parts of IncozolBH latent curing agents, be evacuated to below -0.098Mpa and 20~35 DEG C of high-speed stirreds of temperature control extremely
Material is uniform, and discharging packing is for use after reaching requirement.
Performance test：
1st, surface drying time：It is tested according to 8.2B law regulations in GB/T13477.5-2002..
2nd, curing rate：According to 6.8 regulation test in HG/T4363-2012.
2nd, tensile strength and elongation at break：It is tested according to GB/T528-2009.
3rd, tensile shear strength：HG/T4363-2012 is tested, and controls bondline thickness 2mm, hardening time 168h.
4th, putty plate matches somebody with somebody cementability (room temperature 7d)：Under 23 DEG C, 50% relative humidities, require to modulate according to putty
Putty is mixed, uniformly fluid sealant to surface of steel plate, before the incomplete surface drying of putty, is coated onto putty plate table by blade coating immediately after
Face, applies length about 100mm, width about 10mm, and the adhesive tape of thickness about 5mm uses nipper plier to carry out disbonded test, often after curing 7d
Glue is cut every about 2mm, 80mm is no less than every sample stripping glue length, counts cohesional failure rate, cohesional failure rate gets over high adhesiveness
It can be better.
5th, putty plate cementability (hot and humid 7d)：Under 23 DEG C, 50% relative humidities, require to adjust according to putty
System mixing putty, uniformly fluid sealant to surface of steel plate, before the incomplete surface drying of putty, is coated onto putty plate by blade coating immediately after
Surface applies length about 100mm, width about 10mm, the adhesive tape of thickness about 5mm, adhesive tape once curing or aging in condition successively：
1) 23 DEG C, cure 7d under 50% relative humidities；2) under 70 DEG C, 100% relative humidity after aging 7d again 23 DEG C,
Recover 2h under 50% relative humidity conditions.Disbonded test is carried out using nipper plier, glue is cut every about 2mm, it is long every sample stripping glue
Degree is no less than 80mm, counts cohesional failure rate.
6th, putty plate cementability (soaked 30d)：
Under 23 DEG C, 50% relative humidities, modulation mixing putty is required according to putty, is uniformly scratched immediately after
To surface of steel plate, before the incomplete surface drying of putty, fluid sealant is coated onto putty plate surface, applies length about 100mm, width is about
10mm, the adhesive tape of thickness about 5mm are soaked in 30d in deionized water after curing 7d, are taken out after expiring in 23 DEG C, 50% relative humidity
Under the conditions of recover 2h, using nipper plier carry out disbonded test, cut glue every about 2mm, every sample stripping glue length be no less than
80mm counts cohesional failure rate.
7th, electrophoretic paint plate matches somebody with somebody cementability (room temperature 7d)：Under 23 DEG C, 50% relative humidities, fluid sealant is coated onto electricity
Swimming paint plate surface, applies length about 100mm, width about 10mm, and the adhesive tape of thickness about 5mm is removed after curing 7d using nipper plier
Experiment, glue is cut every about 2mm, is no less than 80mm every sample stripping glue length, is counted cohesional failure rate, cohesional failure rate is got over
High adhesiveness can be better.
8th, electrophoretic paint plate cementability (hot and humid 7d)：
Under 23 DEG C, 50% relative humidities, fluid sealant is coated onto electrophoretic paint plate surface, applies length about 100mm, it is wide
Spend about 10mm, the adhesive tape of thickness about 5mm, adhesive tape once curing or aging in condition successively：1) 23 DEG C, 50% relative humidity item
Cure 7d under part；2) recover again under 23 DEG C, 50% relative humidity conditions after aging 7d under 70 DEG C, 100% relative humidity
2h.Disbonded test is carried out using nipper plier, glue is cut every about 2mm, in sample stripping glue length is no less than 80mm, counts
Poly- destructive rate.
9th, electrophoretic paint plate cementability (soaked 30d)：
Under 23 DEG C, 50% relative humidities, fluid sealant is coated onto electrophoretic paint plate surface, applies length about 100mm, it is wide
Spend about 10mm, the adhesive tape of thickness about 5mm, cure 7d after be soaked in 30d in deionized water, after expiring take out 23 DEG C, 50% relatively
Recover 2h under damp condition, carry out disbonded test using nipper plier, glue is cut every about 2mm, it is many every sample stripping glue length
In 80mm, cohesional failure rate is counted.
10th, high temperature and heavy wet solidification bulge situation：
Square groove is made using polyfluortetraethylene plate, square groove size length × width × height is：200mm × 10mm × 10mm,
Only square groove upper surface open.Under 23 DEG C, 50% relative humidities, fluid sealant is slowly squeezed into square groove and (avoids lacking
Glue causes stomata), the extra glue in square groove upper surface is struck off using scraper plate, is then immediately placed in temperature as 50 DEG C, relatively
The climatic chamber of humidity 100% cures 7d, then takes out, and whether observation adhesive tape upper surface has bulge.Then plastic emitting is removed
Item is along its length splitted adhesive tape using blade, and whether observe on section has stomata.For the fluid sealant that has excellent performance and
Speech, bulge are more few better.
11st, craftsmanship is smoothed out：
Fluid sealant is got on glass plate, then a small amount of hand cleanser aqueous solution is sprayed toward glue surface using watering can, then uses hand
Glue is smeared into regulation face shaping, whether glue easily smoothes out and smooth out whether rear surface glue is present with stream during observing this
Heisui River and stream plain boiled water.Product appearance can be influenced by stream Heisui River and stream plain boiled water phenomenon occur, belong to defective products.
12nd, cured glue film gloss
It is the square framed of 2mm that fluid sealant is squeezed into thickness, is struck off, and stands and cures 7d, then according to GB/T9754-
2007 test its glossiness.The general position gloss for requiring dumb light should be less than 30, should more preferably be less than 25.
13rd, fluid sealant gloss stability after aging
The intact fluid sealant of sealing will be produced and be placed in 60 DEG C of oven ageing 168h, taking-up is cooled to room temperature.Then will
It is the square framed of 2mm that fluid sealant, which squeezes into thickness, is struck off, and stands and cures 7d, then tests its light according to GB/T9754-2007
Pool.For this data compared with the data before aging, variation is the smaller the better.
Embodiment (fluid sealant 1~5) and the specific performance test result of comparative example (fluid sealant 6~9) ginseng are shown in Table 1,
Analytical table 1 is understood：With NCO sealing end unsaturated polyether polyol polyurethane prepolymer (PI-1, PI-2, PI-3) addition,
The adhesive property enhancing of putty plate；Increase with the additive amount of latent curing agent, bulge tails off；Reduce NCO sealing ends polyethers containing EO
The additive amount of polyurethane prepolymer (PE-2), smoothing out craftsmanship can improve.Using or improve the better plasticizer alkyl of compatibility
After phenyl sulfonate Mesamoll, dumb light (glossiness) stability of fluid sealant is more preferable.One pack system prepared by the embodiment of the present invention is wet
Curing urethane fluid sealant, in addition to it can be bonded electrophoretic paint plate, moreover it is possible to resistance to after bonding to the good bonding of putty plate progress
Ageing properties are also very excellent；In addition craftsmanship and dumb light (gloss are smoothed out using also not bulge under hot and humid environment
Degree) stability is also very excellent.
The performance test results of table 1, embodiment fluid sealant 1~5 and comparative example fluid sealant 6~10
The present invention is not limited to the above-described embodiments, for those skilled in the art, is not departing from
On the premise of the principle of the invention, several improvements and modifications can also be made, these improvements and modifications are also considered as the protection of the present invention
Within the scope of.The content not being described in detail in this specification belongs to the prior art well known to professional and technical personnel in the field.
Claims (14)
1. a kind of single-component mist-solidifying polyurethane sealant, it is characterised in that：In parts by mass, the single-component mist-solidifying
Polyurethane sealant includes following components：
The pure PO polyether polyurethane prepolymers of 100 parts of NCO sealing ends, 40~60 parts of NCO sealing ends polyether polyurethane prepolymers containing EO, 1
The unsaturated polyether polyol polyurethane prepolymer of~100 parts of NCO sealing ends, 110~150 parts of plasticizer, 1~2 part silane coupled
Agent, 1~2.5 part of deicer, 1.5~3 parts of crosslinking agents, 150~400 parts of inorganic fillers, 30~60 parts of surface matt modifying agent,
0.2~0.4 part of organic acid catalyst, 0.05~0.4 part of organotin catalysts, 0.5~6 part of thixotropic agent, 5~20 parts of latent curings
Agent.
2. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The NCO sealing ends
Pure PO polyether polyurethane prepolymers reacted by excessive isocyanates and pure PO polyether polyol, catalyst, reaction suppressor
It is made, NCO content is between 2.0~3.0%.
3. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The NCO sealing ends
Unsaturated polyether polyol polyurethane prepolymer by excessive isocyanates and the polyether polyol containing unsaturated double-bond, catalysis
Agent, reaction suppressor reaction are made, and NCO content is between 2.0~3.0%.
4. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The NCO sealing ends
Polyether polyurethane prepolymer containing EO by excessive isocyanates and polyether polyol containing EO, catalyst, reaction suppressor reaction
It is made, NCO content is between 2.0~3.0%.
5. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The plasticizer is
Phenyl alkylsulf, diisononyl phthalate, diisooctyl phthalate, polyadipate second binary alcohol esters, gather oneself two
One or more in acid propylene glycol ester.
6. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：It is described silane coupled
Agent is the one or more in amino coupling agent, sulfydryl coupling agent, epoxy group coupling agent.
7. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The deicer is
Tolysulfonyl isocyanates, 3- butyl -2- (one kind in 1- ethyl pentyl group) oxazolidines, 2- isopropyl -3- oxazolidine ethyl alcohol
It is or a variety of.
8. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The crosslinking agent is
The isocyanates of three or more degrees of functionality.
9. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The inorganic filler
For the inorganic powder of non-surface treated and water content less than 500ppm, type of powder is kaolin, powdered whiting, talcum
One or more in powder, carbon black, silicon powder.
10. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The surface is sub-
Light modifying agent is talcum powder, the one or more in PVC paste resin, polyethylene micropowder.
11. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The organic acid
Catalyst be aliphatic unitary, binary, polybasic carboxylic acid or aromatic carboxylic acid, be maleic acid, fumaric acid, oxalic acid,
One kind in salicylic acid, tartaric acid, malic acid, citric acid, ascorbic acid, acrylic acid, methacrylic acid, benzoic acid, caffeic acid
It is or a variety of.
12. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The latent curing
Agent is aldimine or Polyaldimines latent curing agent.
13. a kind of single-component mist-solidifying polyurethane sealant as described in claim 1, it is characterised in that：The thixotropic agent
For the one or more in hydrophobic fumed silica, polyureas thixotropic agent, polyacrylamide.
14. a kind of a kind of preparation side of single-component mist-solidifying polyurethane sealant as described in claim 1-13 any one
Method, which is characterized in that comprise the following steps：
In 0~25 DEG C of temperature, relative humidity is less than under 40% environment, and the pure PO that 100 parts of NCO sealing ends are added in into glue container gathers
Ether polyurethane prepolymer, 40~60 parts of NCO sealing ends polyether polyurethane prepolymers containing EO, unsaturations of 1~100 part of NCO sealing end are gathered
Ethoxylated polyhydric alcohol polyurethane prepolymer, 110~150 parts of plasticizer, 1~2 part of silane coupling agent, 1~2.5 part of deicer, 1.5~3
Part crosslinking agent, it is stirred below uniform to material to be evacuated to -0.098Mpa；
Nitrogen protects pressure release, adds in 150~400 parts of inorganic fillers and 30~60 parts of surface matt modifying agent, be evacuated to-
Simultaneously 20~35 DEG C of stirrings of temperature control are uniform to material by below 0.098Mpa；
Nitrogen protection pressure release, 0.2~0.4 part of organic acid catalyst of addition, 0.05~0.4 part of organotin catalysts, 0.5~6 part
Thixotropic agent, 5~20 parts of latent curing agents, are evacuated to below -0.098Mpa and 20~35 DEG C of stirrings of temperature control are uniform to material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711433156.9A CN108048025B (en) | 2017-12-26 | 2017-12-26 | Single-component moisture-curing polyurethane sealant and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711433156.9A CN108048025B (en) | 2017-12-26 | 2017-12-26 | Single-component moisture-curing polyurethane sealant and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108048025A true CN108048025A (en) | 2018-05-18 |
| CN108048025B CN108048025B (en) | 2020-09-08 |
Family
ID=62128017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711433156.9A Active CN108048025B (en) | 2017-12-26 | 2017-12-26 | Single-component moisture-curing polyurethane sealant and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108048025B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021910A (en) * | 2018-08-23 | 2018-12-18 | 福建中意铁科新型材料有限公司 | A kind of one-component polyurethane sealant and preparation method thereof |
| CN110684501A (en) * | 2019-09-25 | 2020-01-14 | 郑州骏惠材料技术有限公司 | Polyurethane hard foam powder filled single-component polyurethane sealant and preparation method thereof |
| CN111073587A (en) * | 2019-12-19 | 2020-04-28 | 上海华峰新材料研发科技有限公司 | Ultralow temperature-resistant environment-friendly double-component polyurethane adhesive and preparation and application thereof |
| WO2020201419A1 (en) * | 2019-04-05 | 2020-10-08 | Sika Technology Ag | Moisture-curing composition with good adhesive properties |
| CN112029446A (en) * | 2020-08-04 | 2020-12-04 | 安徽天安新材料有限公司 | PVC adhesive and preparation method and application thereof |
| CN112375200A (en) * | 2020-11-13 | 2021-02-19 | 广东盛业化学科技有限公司 | Low-temperature low-humidity fast-curing polyurethane composition and preparation method thereof |
| CN112694863A (en) * | 2020-12-31 | 2021-04-23 | 湖北回天新材料股份有限公司 | Single-component polyurethane electronic component fixing glue and preparation method and application thereof |
| CN112724911A (en) * | 2020-12-28 | 2021-04-30 | 安徽匠星联创新材料科技有限公司 | Polyurea polyurethane mixed single-component high-back grass gum |
| CN113462342A (en) * | 2021-07-21 | 2021-10-01 | 多利隆人造草坪集团有限公司 | Single-component polyurethane adhesive and preparation method thereof, artificial lawn and construction method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0674404B2 (en) * | 1986-05-30 | 1994-09-21 | 出光石油化学株式会社 | Composition for bonding metal structural materials |
| CN101255327A (en) * | 2008-04-03 | 2008-09-03 | 武汉理工大学 | Preparation method of wet-curing reaction type polyurethane hot melt adhesives for shoes |
| CN102504750A (en) * | 2011-11-22 | 2012-06-20 | 东莞市普赛达密封粘胶有限公司 | Polyurethane sealant with good initial adhesion |
| CN107142068A (en) * | 2017-04-10 | 2017-09-08 | 广东普赛达密封粘胶有限公司 | A kind of heat cure one-component polyurethane compositions and preparation method thereof |
-
2017
- 2017-12-26 CN CN201711433156.9A patent/CN108048025B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0674404B2 (en) * | 1986-05-30 | 1994-09-21 | 出光石油化学株式会社 | Composition for bonding metal structural materials |
| CN101255327A (en) * | 2008-04-03 | 2008-09-03 | 武汉理工大学 | Preparation method of wet-curing reaction type polyurethane hot melt adhesives for shoes |
| CN102504750A (en) * | 2011-11-22 | 2012-06-20 | 东莞市普赛达密封粘胶有限公司 | Polyurethane sealant with good initial adhesion |
| CN107142068A (en) * | 2017-04-10 | 2017-09-08 | 广东普赛达密封粘胶有限公司 | A kind of heat cure one-component polyurethane compositions and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 曹云来: "《密封胶 技术·配方·应用》", 30 September 2001, 化学工业出版社 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021910A (en) * | 2018-08-23 | 2018-12-18 | 福建中意铁科新型材料有限公司 | A kind of one-component polyurethane sealant and preparation method thereof |
| CN113557257A (en) * | 2019-04-05 | 2021-10-26 | Sika技术股份公司 | Moisture-curing composition with good adhesion properties |
| WO2020201419A1 (en) * | 2019-04-05 | 2020-10-08 | Sika Technology Ag | Moisture-curing composition with good adhesive properties |
| CN113557257B (en) * | 2019-04-05 | 2024-01-30 | Sika技术股份公司 | Moisture-curable compositions with good adhesion properties |
| CN110684501A (en) * | 2019-09-25 | 2020-01-14 | 郑州骏惠材料技术有限公司 | Polyurethane hard foam powder filled single-component polyurethane sealant and preparation method thereof |
| CN110684501B (en) * | 2019-09-25 | 2022-03-22 | 郑州大学 | Polyurethane hard foam powder filled single-component polyurethane sealant and preparation method thereof |
| CN111073587A (en) * | 2019-12-19 | 2020-04-28 | 上海华峰新材料研发科技有限公司 | Ultralow temperature-resistant environment-friendly double-component polyurethane adhesive and preparation and application thereof |
| CN111073587B (en) * | 2019-12-19 | 2021-10-29 | 上海华峰新材料研发科技有限公司 | Ultralow temperature-resistant environment-friendly double-component polyurethane adhesive and preparation and application thereof |
| CN112029446A (en) * | 2020-08-04 | 2020-12-04 | 安徽天安新材料有限公司 | PVC adhesive and preparation method and application thereof |
| CN112375200A (en) * | 2020-11-13 | 2021-02-19 | 广东盛业化学科技有限公司 | Low-temperature low-humidity fast-curing polyurethane composition and preparation method thereof |
| CN112724911A (en) * | 2020-12-28 | 2021-04-30 | 安徽匠星联创新材料科技有限公司 | Polyurea polyurethane mixed single-component high-back grass gum |
| CN112724911B (en) * | 2020-12-28 | 2023-03-07 | 安徽匠星联创新材料科技有限公司 | Polyurea polyurethane mixed single-component high-back grass adhesive |
| CN112694863B (en) * | 2020-12-31 | 2022-09-06 | 湖北回天新材料股份有限公司 | Single-component polyurethane electronic component fixing glue and preparation method and application thereof |
| CN112694863A (en) * | 2020-12-31 | 2021-04-23 | 湖北回天新材料股份有限公司 | Single-component polyurethane electronic component fixing glue and preparation method and application thereof |
| CN113462342A (en) * | 2021-07-21 | 2021-10-01 | 多利隆人造草坪集团有限公司 | Single-component polyurethane adhesive and preparation method thereof, artificial lawn and construction method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108048025B (en) | 2020-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108048025A (en) | A kind of single-component mist-solidifying polyurethane sealant and preparation method thereof | |
| CN102115654B (en) | Automobile hemming adhesive and preparation method thereof | |
| US6025416A (en) | Two-component adhesive/sealing mass with high initial adhesiveness | |
| CN106030006B (en) | Easy to apply air and water barrier articles | |
| CN105038681A (en) | Silane modified resin sealing gum and preparing method thereof | |
| RU2420554C2 (en) | Single-component anhydrous coating composition for sealing building structures and flat roofs | |
| CN107109152B (en) | Air and water barrier articles | |
| CN108034352A (en) | Modified silicone seal gum silane coupling agent suitable for PC buildings and preparation method thereof | |
| CN105885766B (en) | A kind of environment-friendly high-intensity nail-free glue and preparation method thereof without organotin | |
| CN108047923A (en) | Assembled architecture modified silicone seal gum primary coat liquid and preparation method thereof | |
| CN107216845A (en) | A kind of environment-friendly type end siloxy group polyurethane sealant and preparation method thereof | |
| CN110157376A (en) | Transparent two-component silane modified polyether seal glue and preparation method thereof | |
| JP5632607B2 (en) | Protective covering material for concrete structure and method for protecting concrete structure | |
| EP1724321A1 (en) | Solventless adhesive and sealant | |
| CN104870506B (en) | Adhesive suitable for installing vehicle window | |
| CN107011855A (en) | Normal temperature cure sealant composition and preparation method thereof | |
| GB2454584A (en) | Sealant composition | |
| CN111574951B (en) | Self-skinning modified polyurethane thermosetting sealant composition and preparation method thereof | |
| CN106497486A (en) | Low-temperature curable double-component silane modified polyether seal glue and preparation method thereof | |
| WO2007093381A1 (en) | One-component, solvent free contact adhesive | |
| CN107531865A (en) | Reactive polyurethanes plasticiser and adhesive prepared therefrom | |
| CN105111991A (en) | High strength silane-modified polyether wall glue and preparation method therefor | |
| CN103087669B (en) | Moisture-curing polyurethane hot-melt adhesive for manufacturing of composite boards | |
| CN108587545A (en) | A kind of single component silane modified polyether seal glue and preparation method thereof for ALC plates | |
| CN108102607A (en) | A kind of silane-modified adhesive of fast surface drying speed location high-strength and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |