CN110591640A - Low-VOC (volatile organic compound) indoor joint filling sealant - Google Patents
Low-VOC (volatile organic compound) indoor joint filling sealant Download PDFInfo
- Publication number
- CN110591640A CN110591640A CN201910827826.8A CN201910827826A CN110591640A CN 110591640 A CN110591640 A CN 110591640A CN 201910827826 A CN201910827826 A CN 201910827826A CN 110591640 A CN110591640 A CN 110591640A
- Authority
- CN
- China
- Prior art keywords
- parts
- low
- epoxy
- amine
- terminated
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/458—Block-or graft-polymers containing polysiloxane sequences containing polyurethane sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
- C08G83/006—After treatment of hyperbranched macromolecules
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/10—Block or graft copolymers containing polysiloxane sequences
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a low-VOC indoor joint filling sealant which is characterized by comprising the following components in parts by weight: 25-35 parts of isocyanatopropyl triethoxy silane modified hyperbranched polyglycidyl ether, 40-60 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 10-15 parts of filler, 2-5 parts of plasticizer, 0.5-1.5 parts of dispersant and 1-2 parts of defoaming agent. The invention also discloses a preparation method of the low VOC indoor joint filling sealant. The low-VOC indoor joint filling sealant disclosed by the invention is excellent in comprehensive performance, environment-friendly performance, flame retardance and storage stability, high in bonding strength, good in joint filling effect, high in safety, strong in weather resistance, excellent in ageing resistance, low in cost, free of pollution and long in service life.
Description
Technical Field
The invention relates to the technical field of sealants, in particular to a low-VOC indoor joint filling sealant.
Background
With the progress of society and the development of science and technology, building materials are also rapidly developed, and the market demand is increased year by year. The quality of the performance of the building materials directly influences the normal use and the service life of the buildings and the structures, and also influences the visual effect of indoor decoration. The sealant is a common building material, and is particularly used in the indoor decoration process, such as the bonding between wall boards, crack filling and pit slot repairing, which all need to be utilized.
The sealing glue is a sealing material which deforms along with the shape of the sealing surface, is not easy to flow and has certain cohesiveness. It is a flowable or extrudable amorphous material which fills and seals the seam and is gradually set into a plastic solid, viscoelastic or elastic sealant by drying, temperature change, solvent evaporation, chemical crosslinking and stable bonding to the substrate. The joint filling sealant is one of a plurality of sealants, and the performance of the joint filling sealant directly influences the joint filling effect and the quality of construction engineering, so that the development of the joint filling sealant with excellent performance is significant.
At present, common sealant is solvent type sealant, the solvent type sealant usually contains a large amount of volatile organic solvents, the organic solvents are volatilized in the curing process of the sealant or enter indoor air to influence the air quality, and the content of the volatile organic solvents, namely the VOC content, is an important index for representing the indoor air quality. Too high a VOC content not only pollutes the environment but also causes harm to the constructors. With the enhancement of environmental awareness of people and the successive emergence of laws and regulations of national and local governments, the low-VOC indoor joint sealing sealant becomes the mainstream direction for the development of the sealant industry at present and even in a period of time in the future, and has very high market potential power.
The silane modified polyether (MS) sealant is a high-performance environment-friendly sealant prepared by taking polyether resin terminated by alkoxy silane as a base material. The main chain of the silane modified polyether resin is of a macromolecular ether chain structure, so that good flexibility and high extensibility can be provided; and the end group is a siloxy group, and is in contact with moisture and then undergoes a hydrolytic condensation reaction to form a-Si-O-Si-three-dimensional space network structure. Therefore, the MS sealant has the advantages of excellent weather resistance, durability, cohesiveness, paintability, high deformation displacement resistance, no pollution, low VOC content, easy construction and the like. However, the MS sealant in the prior art has the problems of poor flame retardance, weather resistance and aging resistance and the like.
The application publication number CN 107523256A of Chinese invention discloses an aqueous elastic fireproof joint sealing sealant and a preparation method thereof, and the aqueous elastic fireproof joint sealing sealant comprises the following components in parts by weight: 50-70 parts of organic silicon emulsion, 20-30 parts of acrylic waterproof emulsion, 10-20 parts of composite flame retardant, 10-20 parts of filler, 0.5-1 part of rheological agent, 1-2 parts of defoaming agent, 0.5-1.5 parts of dispersing agent and 2-4 parts of tackifier, wherein the composite flame retardant is mainly prepared from magnesium salt, nano montmorillonite and carbon nano tube. The sealant has excellent flame retardance and environmental protection performance. However, the comprehensive performance, the bonding performance and the weather resistance of the composite material are further to be improved, the compatibility among the components is worthy of improvement, and the performance stability has a certain improvement space.
Therefore, the development of the low-VOC indoor joint sealing sealant with excellent comprehensive performance, environmental protection performance, flame retardance, storage stability and weather resistance, high bonding strength, good joint sealing effect and long service life meets the market demand, has wide market value and application prospect, and has very important significance for promoting the development of the joint sealing sealant industry.
Disclosure of Invention
The invention mainly aims to provide a low-VOC indoor joint filling sealant and a preparation method thereof, wherein the preparation method is simple and easy to operate, the process is easy to control, the environmental pollution is small, the energy consumption in the implementation process is low, and the preparation efficiency and the finished product qualification rate are high; the prepared low-VOC indoor joint filling sealant has the advantages of excellent comprehensive performance, good environmental protection performance, flame retardance and storage stability, high bonding strength, good joint filling effect, high safety, strong weather resistance, excellent ageing resistance, low cost, no pollution and long service life.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows: the low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 25-35 parts of isocyanatopropyl triethoxy silane modified hyperbranched polyglycidyl ether, 40-60 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 10-15 parts of filler, 2-5 parts of plasticizer, 0.5-1.5 parts of dispersant and 1-2 parts of defoaming agent.
Further, the antifoaming agent is one or more of tributyl phosphate, antifoaming agent dele 3100 and antifoaming agent BYK 088.
Further, the dispersing agent is sodium hexametaphosphate and/or sodium polycarboxylate.
Further, the plasticizer is one or a mixture of more than two of simethicone, dibutyl phthalate, dioctyl phthalate, pentachlorodiphenyl and chlorinated paraffin.
Further, the filler is one or more of carbon black, white carbon black, organic bentonite, activated calcium, talcum powder and kaolin.
Further, the preparation method of the amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate comprises the following steps:
adding amine-terminated polyurethane and epoxy-terminated silicone oil into an organic solvent, stirring and reacting for 6-8 hours at the temperature of 80-90 ℃, and then removing the solvent by rotary evaporation to obtain the amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate.
Preferably, the mol ratio of the amine-terminated polyurethane to the epoxy-terminated silicone oil to the organic solvent is 1:1 (6-10).
Preferably, the organic solvent is one of isopropanol, acetone, and N, N-dimethylformamide.
Preferably, the amine-terminated polyurethane is prepared in advance, and has a number average molecular weight of 6200, and the preparation method refers to: the research on the synthesis of amino-terminated polyurethane and the toughening of epoxy resin, the establishment of the country and the like, the science and engineering of high polymer materials, 2005,21(1): 117-.
Preferably, the epoxy-terminated silicone oil is prepared in advance, and the preparation method refers to embodiment 1 of the Chinese patent CN 201610828111.0.
Preferably, the hyperbranched polyglycidyl ether is hyperbranched polyglycidyl ether for four generations, and the preparation method thereof is not particularly limited.
Further, the preparation method of the isopropyltriethoxysilane-modified hyperbranched polyglycidyl ether comprises the following steps: adding the isocyanatopropyl triethoxysilane, the hyperbranched polyglycidyl ether and the catalyst into N-methyl pyrrolidone, stirring and reacting for 6-8 hours at the temperature of 110-120 ℃, cooling to room temperature, and performing rotary evaporation to remove the N-methyl pyrrolidone to obtain the isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether.
Preferably, the mass ratio of the isocyanatopropyltriethoxysilane to the hyperbranched polyglycidyl ether to the catalyst to the N-methylpyrrolidone is 1 (3-5) to (0.2-0.5) to (15-20).
Preferably, the catalyst is selected from at least one of triethylene diamine, N-alkyl morphanthine and dibutyl tin dilaurate.
Further, the preparation method of the low-VOC indoor joint sealing sealant comprises the following steps: adding the components into a kneader according to the proportion, and stirring for 1-3 hours at the temperature of 20-40 ℃; then vacuumizing and heating to slowly raise the temperature to 45-55 ℃, keeping the vacuum degree at-0.08 +/-0.01 Mpa, and stirring for 1-2 hours under heat preservation to obtain the low VOC indoor joint sealing glue.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the low-VOC indoor joint filling sealant provided by the invention is simple and easy to operate in preparation method, easy to control process, low in environmental pollution, low in energy consumption in implementation process, high in preparation efficiency and finished product qualification rate, low in requirements on equipment and reaction conditions, and suitable for large-scale production.
(2) The low-VOC indoor joint filling sealant provided by the invention overcomes the technical problems of high VOC content, large environmental pollution and large harm to human health of the traditional solvent type sealant, overcomes the defects of unsatisfactory flame retardance, weather resistance and aging resistance and the like of the MS sealant in the prior art, and has the advantages of excellent comprehensive performance, environmental protection performance, good flame retardance and storage stability, high bonding strength, good joint filling effect, high safety, strong weather resistance, excellent aging resistance, low cost, no pollution and long service life.
(3) The low VOC indoor joint filling sealant provided by the invention has the advantages that the added components have strong hydrophilic capability,
the added isopropyltriethoxysilane modified hyperbranched polyglycidyl ether has high bonding capability and good compatibility with other components because of containing more active hydroxyl groups and ether groups and a special supermolecular polymer structure, and the added isopropyltriethoxysilane modified hyperbranched polyglycidyl ether has a three-dimensional network structure formed by introducing the ethoxysilicon through modification and performing a crosslinking reaction with the added hydroxyl groups on the amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate in a curing stage, thereby being beneficial to improving the comprehensive performance and the yellowing performance.
(4) According to the low-VOC indoor joint filling sealant provided by the invention, the addition of the amine-terminated polyurethane/end epoxy-terminated silicone oil polycondensate combines the advantages of polyurethane and organic silicon adhesives, so that the comprehensive performance is better, the added filler can further improve the mechanical strength of the sealant, and the joint filling effect is good.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art. The raw materials in the embodiment of the invention are all purchased commercially; the amino-terminated polyurethane is prepared in advance, the number average molecular weight is 6200, and the preparation method refers to the following steps: the synthesis of amino-terminated polyurethane and the research of toughening epoxy resin, the establishment of the country and the like, the science and engineering of high polymer materials, 2005,21(1): 117-; the epoxy-terminated silicone oil is prepared in advance, and the preparation method refers to embodiment 1 of Chinese invention patent CN 201610828111.0; the hyperbranched polyglycidyl ether is hyperbranched polyglycidyl ether for four generations, and the preparation method is not particularly limited.
Example 1
The low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 25 parts of isocyanatopropyl triethoxy silane modified hyperbranched polyglycidyl ether, 40 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 10 parts of carbon black, 2 parts of dimethyl silicone oil, 0.5 part of sodium hexametaphosphate and 1 part of tributyl phosphate.
The preparation method of the amine-terminated polyurethane/epoxy-terminated silicon oil polycondensate comprises the following steps: adding amine-terminated polyurethane and end epoxy silicone oil into isopropanol, stirring and reacting for 6 hours at 80 ℃, and then performing rotary evaporation to remove the solvent to obtain an amine-terminated polyurethane/end epoxy silicone oil polycondensate; the mol ratio of the amine-terminated polyurethane to the epoxy-terminated silicone oil to the isopropanol is 1:1: 6.
The preparation method of the isopropyltriethoxysilane modified hyperbranched polyglycidyl ether comprises the following steps: adding 10g of isocyanatopropyl triethoxysilane, 30g of hyperbranched polyglycidyl ether and 2g of triethylene diamine into 150g of N-methylpyrrolidone, stirring and reacting at 110 ℃ for 6 hours, cooling to room temperature, and performing rotary evaporation to remove N-methylpyrrolidone, thereby obtaining the isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether.
The preparation method of the low VOC indoor joint filling sealant comprises the following steps: adding the components into a kneader according to the proportion, and stirring for 1 hour at the temperature of 20 ℃; and then vacuumizing and heating to slowly raise the temperature to 45 ℃, keeping the vacuum degree at minus 0.08 +/-0.01 Mpa, and stirring for 1 hour under heat preservation to obtain the low-VOC indoor joint sealing sealant.
Example 2
The low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 27 parts of isocyanatopropyl triethoxy silane modified hyperbranched polyglycidyl ether, 45 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 12 parts of white carbon black, 3 parts of dibutyl phthalate, 0.7 part of sodium polycarboxylate and 31001.2 parts of defoaming agent.
The preparation method of the amine-terminated polyurethane/epoxy-terminated silicon oil polycondensate comprises the following steps: adding amine-terminated polyurethane and end epoxy silicone oil into acetone, stirring and reacting for 6.5 hours at 83 ℃, and then performing rotary evaporation to remove the solvent to obtain an amine-terminated polyurethane/end epoxy silicone oil polycondensate; the mol ratio of the amine-terminated polyurethane to the epoxy-terminated silicone oil to the acetone is 1:1 (6-10).
The preparation method of the isopropyltriethoxysilane modified hyperbranched polyglycidyl ether comprises the following steps: adding 10g of isocyanatopropyltriethoxysilane, 35g of hyperbranched polyglycidyl ether and 3g of N-alkyl morphanthine into 170g of N-methylpyrrolidone, stirring and reacting at 113 ℃ for 6.5 hours, cooling to room temperature, and performing rotary evaporation to remove the N-methylpyrrolidone to obtain the isocyanatopropyltriethoxysilane modified hyperbranched polyglycidyl ether.
The preparation method of the low VOC indoor joint filling sealant comprises the following steps: adding the components into a kneader according to the proportion, and stirring for 1.5 hours at 25 ℃; then vacuumizing and heating to slowly raise the temperature to 48 ℃, keeping the vacuum degree at minus 0.08 +/-0.01 Mpa, and stirring for 1.3 hours under heat preservation to obtain the low VOC indoor joint sealing glue.
Example 3
The low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 30 parts of isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether, 50 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 13 parts of organic bentonite, 3.5 parts of dioctyl phthalate, 0.9 part of sodium hexametaphosphate and BYK0881.5 parts of defoaming agent.
The preparation method of the amine-terminated polyurethane/epoxy-terminated silicon oil polycondensate comprises the following steps: adding amine-terminated polyurethane and epoxy-terminated silicone oil into N, N-dimethylformamide, stirring and reacting for 7 hours at 85 ℃, and then performing rotary evaporation to remove the solvent to obtain an amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate; the mol ratio of the amine-terminated polyurethane to the epoxy-terminated silicone oil to the N, N-dimethylformamide is 1:1 (6-10).
The preparation method of the isopropyltriethoxysilane modified hyperbranched polyglycidyl ether comprises the following steps: adding 10g of isocyanatopropyl triethoxysilane, 40g of hyperbranched polyglycidyl ether and 4g of dibutyltin dilaurate into 185g of N-methylpyrrolidone, stirring and reacting at 115 ℃ for 7 hours, cooling to room temperature, and performing rotary evaporation to remove the N-methylpyrrolidone, thereby obtaining the isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether.
The preparation method of the low VOC indoor joint filling sealant comprises the following steps: adding the components into a kneader according to the proportion, and stirring for 2 hours at the temperature of 30 ℃; then vacuumizing and heating to slowly raise the temperature to 50 ℃, keeping the vacuum degree at minus 0.08 +/-0.01 Mpa, and stirring for 1.5 hours under heat preservation to obtain the low VOC indoor joint sealing glue.
Example 4
The low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 34 parts of isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether, 58 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 14 parts of filler, 4.5 parts of plasticizer, 1.4 parts of dispersant and 1.8 parts of defoaming agent.
The defoaming agent is formed by mixing tributyl phosphate, a defoaming agent Demodex 3100 and a defoaming agent BYK088 according to the mass ratio of 1:2: 3; the dispersing agent is formed by mixing sodium hexametaphosphate and sodium polycarboxylate according to the mass ratio of 3: 5; the plasticizer is formed by mixing dimethyl silicone oil, dibutyl phthalate, dioctyl phthalate, pentachlorodiphenyl and chlorinated paraffin according to the mass ratio of 1:2:4:5: 3; the filler is formed by mixing carbon black, white carbon black, organic bentonite, active calcium, talcum powder and kaolin according to the mass ratio of 1:3:2:2:3: 5.
The preparation method of the amine-terminated polyurethane/epoxy-terminated silicon oil polycondensate comprises the following steps: adding amine-terminated polyurethane and end epoxy silicone oil into isopropanol, stirring and reacting for 7.5 hours at 88 ℃, and then performing rotary evaporation to remove the solvent to obtain an amine-terminated polyurethane/end epoxy silicone oil polycondensate; the mol ratio of the amine-terminated polyurethane to the epoxy-terminated silicone oil to the isopropanol is 1:1: 9;
the preparation method of the isopropyltriethoxysilane modified hyperbranched polyglycidyl ether comprises the following steps: adding 10g of isocyanatopropyltriethoxysilane, 48g of hyperbranched polyglycidyl ether and 4.8g of catalyst into 195g of N-methylpyrrolidone, stirring and reacting at 118 ℃ for 7.8 hours, cooling to room temperature, and performing rotary evaporation to remove the N-methylpyrrolidone to obtain isocyanatopropyltriethoxysilane modified hyperbranched polyglycidyl ether; the catalyst is prepared by mixing triethylene diamine, N-alkyl morphanthine and dibutyltin dilaurate according to the mass ratio of 1:3: 5.
The preparation method of the low VOC indoor joint filling sealant comprises the following steps: adding the components into a kneader according to the mixture ratio, and stirring for 2.8 hours at 38 ℃; then vacuumizing and heating to slowly raise the temperature to 53 ℃, keeping the vacuum degree at minus 0.08 +/-0.01 Mpa, and stirring for 1.9 hours under heat preservation to obtain the low VOC indoor joint sealing glue.
Example 5
The low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 35 parts of isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether, 60 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 15 parts of talcum powder, 5 parts of chlorinated paraffin, 1.5 parts of sodium polycarboxylate and 2 parts of tributyl phosphate.
The preparation method of the amine-terminated polyurethane/epoxy-terminated silicon oil polycondensate comprises the following steps: adding amine-terminated polyurethane and epoxy-terminated silicone oil into N, N-dimethylformamide, stirring and reacting for 8 hours at 90 ℃, and then performing rotary evaporation to remove the solvent to obtain an amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate; the mol ratio of the amine-terminated polyurethane to the epoxy-terminated silicone oil to the N, N-dimethylformamide is 1:1: 10.
The preparation method of the isopropyltriethoxysilane modified hyperbranched polyglycidyl ether comprises the following steps: adding 10g of isocyanatopropyltriethoxysilane, 50g of hyperbranched polyglycidyl ether and 5g of N-alkyl morphanthine into 200g of N-methylpyrrolidone, stirring and reacting at 120 ℃ for 8 hours, cooling to room temperature, and performing rotary evaporation to remove the N-methylpyrrolidone to obtain the isocyanatopropyltriethoxysilane modified hyperbranched polyglycidyl ether.
The preparation method of the low VOC indoor joint filling sealant comprises the following steps: adding the components into a kneader according to the proportion, and stirring for 3 hours at 40 ℃; and then vacuumizing and heating to slowly raise the temperature to 55 ℃, keeping the vacuum degree at minus 0.08 +/-0.01 Mpa, and stirring for 2 hours under heat preservation to obtain the low-VOC indoor joint sealing glue.
Comparative example 1
This example provides a low VOC indoor joint sealant substantially the same as example 1 except that no isocyanatopropyltriethoxysilane-modified hyperbranched polyglycidyl ether is added in step S4.
Comparative example 2
This example provides a low VOC indoor joint sealant substantially the same as example 1 except that no amine-terminated polyurethane/epoxy-terminated silicone oil condensation polymer is added in step S4.
Comparative example 3
This example provides a low VOC indoor caulking sealant substantially the same as example 1 except that no carbon black is added in step S4.
Comparative example 4
This example provides a commercially available indoor joint sealant comprising silicone as the major component.
To further illustrate the beneficial technical effects of the sealants according to the embodiments of the present invention, the sealants described in examples 1-5 and comparative examples 1-4 above were tested for performance, and the test results and test methods are shown in table 1.
TABLE 1
As can be seen from Table 1, the light transmittance of the low VOC indoor joint filling sealant disclosed by the embodiment of the invention is more than or equal to 98.9%, the tensile strength is more than or equal to 4.40MPa, the volatile organic compounds are less than or equal to 25g/L, and the fixed-elongation adhesion property is not damaged and no yellowing is generated; the light transmittance of the low-VOC indoor joint filling sealant in the comparative example is less than or equal to 98.0 percent, the tensile strength is less than or equal to 4.03MPa, the volatile organic compounds are more than or equal to 15g/L, and the fixed-elongation caking property is not damaged but yellowing occurs. Therefore, the synergistic effect of the isocyanatopropyltriethoxysilane modified hyperbranched polyglycidyl ether and the amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate greatly contributes to the improvement of the light transmittance, the tensile strength, the definite-elongation caking property and the yellowing property of the sealant, and the VOC content can be effectively reduced; the mechanical property of the sealant can be effectively improved by adding the filler; by comparison, the low-VOC indoor joint filling sealant is superior to the commercial products in the aspects of tensile strength, transparency, caking property, yellowing property, environmental protection property and the like.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The low-VOC indoor joint filling sealant is characterized by comprising the following components in parts by weight: 25-35 parts of isocyanatopropyl triethoxy silane modified hyperbranched polyglycidyl ether, 40-60 parts of amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate, 10-15 parts of filler, 2-5 parts of plasticizer, 0.5-1.5 parts of dispersant and 1-2 parts of defoaming agent.
2. The low VOC indoor caulking sealant according to claim 1, wherein the antifoaming agent is one or more of tributyl phosphate, antifoaming agent hume 3100, antifoaming agent BYK 088.
3. The low VOC indoor caulking sealant according to claim 1, wherein said dispersant is sodium hexametaphosphate and/or sodium polycarboxylate.
4. The low VOC indoor caulking sealant according to claim 1, wherein the plasticizer is one or a mixture of more than two of simethicone, dibutyl phthalate, dioctyl phthalate, pentachlorodiphenyl and chlorinated paraffin.
5. The low VOC indoor caulking sealant according to claim 1, wherein the filler is one or more of carbon black, white carbon black, organic bentonite, activated calcium, talcum powder and kaolin.
6. The low VOC indoor caulking sealant according to claim 1, wherein the preparation method of the amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate comprises the following steps: adding amine-terminated polyurethane and epoxy-terminated silicone oil into an organic solvent, stirring and reacting for 6-8 hours at the temperature of 80-90 ℃, and then removing the solvent by rotary evaporation to obtain the amine-terminated polyurethane/epoxy-terminated silicone oil polycondensate.
7. The low VOC indoor caulking sealant according to claim 6, wherein the mol ratio of the amine-terminated polyurethane, the epoxy-terminated silicone oil and the organic solvent is 1:1 (6-10); the organic solvent is one of isopropanol, acetone and N, N-dimethylformamide.
8. The low VOC indoor joint sealant according to claim 1, wherein the preparation method of the isocyanatopropyltriethoxysilane modified hyperbranched polyglycidyl ether comprises the following steps: adding the isocyanatopropyl triethoxysilane, the hyperbranched polyglycidyl ether and the catalyst into N-methyl pyrrolidone, stirring and reacting for 6-8 hours at the temperature of 110-120 ℃, cooling to room temperature, and performing rotary evaporation to remove the N-methyl pyrrolidone to obtain the isocyanatopropyl triethoxysilane modified hyperbranched polyglycidyl ether.
9. The low VOC indoor joint sealant of claim 8, wherein the mass ratio of the isocyanatopropyltriethoxysilane, the hyperbranched polyglycidyl ether, the catalyst and the N-methylpyrrolidone is 1 (3-5): 0.2-0.5): 15-20; the catalyst is at least one of triethylene diamine, N-alkyl morphanthine and dibutyltin dilaurate.
10. The low VOC indoor caulking sealant according to any one of claims 1 to 9, wherein the method for preparing the low VOC indoor caulking sealant comprises the steps of: adding the components into a kneader according to the proportion, and stirring for 1-3 hours at the temperature of 20-40 ℃; then vacuumizing and heating to slowly raise the temperature to 45-55 ℃, keeping the vacuum degree at-0.08 +/-0.01 Mpa, and stirring for 1-2 hours under heat preservation to obtain the low VOC indoor joint sealing glue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910827826.8A CN110591640A (en) | 2019-09-03 | 2019-09-03 | Low-VOC (volatile organic compound) indoor joint filling sealant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910827826.8A CN110591640A (en) | 2019-09-03 | 2019-09-03 | Low-VOC (volatile organic compound) indoor joint filling sealant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110591640A true CN110591640A (en) | 2019-12-20 |
Family
ID=68857384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910827826.8A Pending CN110591640A (en) | 2019-09-03 | 2019-09-03 | Low-VOC (volatile organic compound) indoor joint filling sealant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110591640A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114456729A (en) * | 2022-02-09 | 2022-05-10 | 浙江荣泰电工器材股份有限公司 | High-temperature-resistant reusable mica tape and preparation method thereof |
| CN118006280A (en) * | 2024-04-08 | 2024-05-10 | 山东广亚新材料有限公司 | Organosilicon modified polyurethane sealant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101410438A (en) * | 2006-01-27 | 2009-04-15 | 莫门蒂夫性能材料股份有限公司 | Low VOC epoxy silane oligomer and compositions containing same |
| CN106432735A (en) * | 2016-09-18 | 2017-02-22 | 安徽科光新材料有限公司 | Double-terminated epoxy silicone oil and preparation method thereof |
| WO2019057670A1 (en) * | 2017-09-20 | 2019-03-28 | Sika Technology Ag | Compositions based on silane-terminated polymers with improved adhesion on thermoplastics |
-
2019
- 2019-09-03 CN CN201910827826.8A patent/CN110591640A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101410438A (en) * | 2006-01-27 | 2009-04-15 | 莫门蒂夫性能材料股份有限公司 | Low VOC epoxy silane oligomer and compositions containing same |
| CN106432735A (en) * | 2016-09-18 | 2017-02-22 | 安徽科光新材料有限公司 | Double-terminated epoxy silicone oil and preparation method thereof |
| WO2019057670A1 (en) * | 2017-09-20 | 2019-03-28 | Sika Technology Ag | Compositions based on silane-terminated polymers with improved adhesion on thermoplastics |
Non-Patent Citations (1)
| Title |
|---|
| 孙涛等: "端氨基聚氨酯的合成及增韧环氧树脂的研究", 《高分子材料科学与工程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114456729A (en) * | 2022-02-09 | 2022-05-10 | 浙江荣泰电工器材股份有限公司 | High-temperature-resistant reusable mica tape and preparation method thereof |
| CN114456729B (en) * | 2022-02-09 | 2023-05-30 | 浙江荣泰电工器材股份有限公司 | High-temperature-resistant and reusable mica tape and preparation method thereof |
| CN118006280A (en) * | 2024-04-08 | 2024-05-10 | 山东广亚新材料有限公司 | Organosilicon modified polyurethane sealant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107541179A (en) | A kind of compound silicone sealant of high-gas resistance performance and preparation method thereof | |
| CN112322250A (en) | Silicone weather-resistant flame-retardant sealant and preparation method thereof | |
| CN107488435A (en) | A kind of high resiliency one-component silicone sealant and preparation method thereof | |
| CN104263315B (en) | A kind of acid transparent silicone weather proofing sealant for building | |
| CN110591640A (en) | Low-VOC (volatile organic compound) indoor joint filling sealant | |
| CN109054715B (en) | Modified silane sealant for LED backlight source and preparation method thereof | |
| CN113512393A (en) | Soaking-resistant flame-retardant single-component silane modified polyether sealant and preparation method thereof | |
| CN116083043B (en) | High-performance sealant and preparation method and application thereof | |
| CN1810907A (en) | Sealing silicone glue with low moisture permeability for hollow glass and its production process | |
| CN105950102B (en) | Hollow glass high elastic recovery rate silicone sealant and preparation method thereof | |
| CN110591639A (en) | Transparent sealant and preparation method thereof | |
| CN113337245A (en) | Dealcoholized photovoltaic module sealant and preparation method thereof | |
| CN114262600A (en) | Low-water-vapor-permeability silicone sealant | |
| CN112980375A (en) | Single-component silane modified polyether sealant and preparation method thereof | |
| CN113308186B (en) | Flame-retardant silane modified waterproof coating and preparation method thereof | |
| CN112521867B (en) | Low-modulus high-elasticity two-component silane modified polyether sealant and preparation method thereof | |
| CN114874744A (en) | Mildew-proof beauty glue for interior decoration and preparation method thereof | |
| CN108314989B (en) | Sealant for purifying air-conditioning air duct and preparation method thereof | |
| CN112210341B (en) | Double-vulcanization system building sealant and preparation method thereof | |
| CN106190013A (en) | A kind of double glazing silicone type bicomponent elastic silicone sealant and preparation method thereof | |
| CN111592850B (en) | Modified silane adhesive and preparation method and application thereof | |
| CN112029408A (en) | Environment-friendly waterproof coating and preparation method thereof | |
| CN103740322A (en) | Inflaming retarding type solar photovoltaic module sealant | |
| CN112680163A (en) | Single-component modified silicone flame-retardant sealant and preparation method thereof | |
| CN110922940B (en) | Environment-friendly MS sealant with rapid solidification and stable storage at room temperature 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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191220 |