CN110551480A - High-performance polyurethane caulking glue and preparation method thereof - Google Patents
High-performance polyurethane caulking glue and preparation method thereof Download PDFInfo
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- CN110551480A CN110551480A CN201910923726.5A CN201910923726A CN110551480A CN 110551480 A CN110551480 A CN 110551480A CN 201910923726 A CN201910923726 A CN 201910923726A CN 110551480 A CN110551480 A CN 110551480A
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3802—Low-molecular-weight compounds having heteroatoms other than oxygen having halogens
- C08G18/3814—Polyamines
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3855—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur
- C08G18/3857—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur having nitrogen in addition to sulfur
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
-
- 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
Abstract
The invention relates to a high-performance polyurethane caulking compound and a preparation method thereof, belonging to the technical field of polyurethane. The high-performance polyurethane caulking compound comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1-5:1, the component A comprises polyether polyol, a filler, a plasticizer, a chain extender, an ultraviolet absorbent, an antioxidant, a catalyst, a defoaming agent and a base material wetting agent, and the component B comprises polyether polyol, isocyanate and a latent curing agent. The polyether polyol has a functionality of 2-3 and a number average molecular weight of 300-4000. The high-performance polyurethane caulking glue disclosed by the invention has the advantages of excellent physical properties, good elasticity, no foaming, aging resistance, low viscosity of feed liquid and good fluidity; the invention also provides a simple and feasible preparation method.
Description
Technical Field
The invention relates to a high-performance polyurethane caulking compound and a preparation method thereof, belonging to the technical field of polyurethane.
Background
At present, caulking glue products in the market mainly comprise polyurethanes, silicones, acrylics and the like, wherein the silicones have good acid-base resistance, strength and the like, but have large smell during construction and great harm to the surrounding environment and constructors. The acrylic acid product has high strength, but has poor flexibility and extensibility, and is easy to crack due to the change of expansion and contraction of the cement expansion joint. The molecular structure of the polyurethane product is a block copolymer combining a soft chain segment and a rigid chain segment, so that the polyurethane product can simultaneously have strength and flexibility. Polyurethane caulking glue is divided into a single component and a double component, and the single component product has gas emission due to the reaction of isocyanate and water, so that foaming and bulging can be avoided, and the strength is reduced. The two-component product is mainly the reaction of isocyanate and polyether polyol, but due to the difference of reaction rate, a small amount of water preferentially participates in the reaction, so that the foaming and bulging defects are difficult to avoid.
Patent CN201410781201.X discloses a polyurethane bi-component material for plastic place expansion joint and a preparation method thereof, the bi-component caulking compound prepared by the bi-component caulking compound improves the product strength and the cohesiveness and reduces the influence of the environmental humidity on the bi-component caulking compound, but according to the design characteristics of a formula system, the viscosity of feed liquid is large, the fluidity is poor, the gap space can not be completely filled during construction, the gap filling effect and the performance are reduced, a trowel is required to be used for trowelling after filling, and the construction difficulty is indirectly increased.
Therefore, a caulking compound product which has excellent physical properties such as tensile elasticity and the like, has low viscosity, strong cohesiveness, no foaming or micro foaming, aging resistance and environmental protection and can be suitable for a humid environment is urgently needed in the market.
Disclosure of Invention
The invention aims to solve the technical problems that the defects in the prior art are overcome, and the high-performance polyurethane caulking glue is provided, has excellent physical properties, is not foamed and ageing-resistant, and has low material liquid viscosity and good fluidity; the invention also provides a simple and feasible preparation method.
The high-performance polyurethane caulking compound comprises a component A and a component B, wherein the mass ratio of the component A6 to the component B is 1-5:1, wherein,
The component A comprises the following raw materials in percentage by mass:
the component B comprises the following raw materials in percentage by mass:
Polyether polyol 60-80%
10-40% of isocyanate
0.5 to 2 percent of latent curing agent;
The polyether polyol has a functionality of 2-3 and a number average molecular weight of 300-4000.
Preferably, the polyether polyol is one or more of MN-3050, DL-3000, DL-1000, DL-400 or DV 125.
preferably, the filler is one or both of 400 mesh talc powder and 600 mesh talc powder.
Preferably, the plasticizer is one or more of dibutyl phthalate, dioctyl phthalate or dimethyl adipate.
preferably, the chain extender is one or two of MOCA and 3, 5-dimethylthiotoluenediamine (DMTDA); the ultraviolet absorbent is 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole.
Preferably, the antioxidant is isooctyl 3, 5-di-tert-butyl-4-hydroxy phenylpropionate.
Preferably, the catalyst is dibutyltin dilaurate.
Preferably, the defoaming agent is one or two of BYK-A506 or BYK-A5356 of BYK chemical company of Germany.
Preferably, the substrate wetting agent is BYK-307 or BYK-344 from BYK Chemicals, Germany.
Preferably, the latent curing agent is Incorez HP from Incorez, uk.
the isocyanate is one or more of MDI-50, MDI-100 or liquefied MDI.
the preparation method of the high-performance polyurethane caulking compound comprises the following steps:
(1) the component A comprises: firstly, putting polyether polyol, a filler, a plasticizer and a chain extender in a formula ratio into a kettle, uniformly stirring, heating to 85-90 ℃, dehydrating under the condition of vacuum degree of-0.1 MPa to ensure that the water content is below 0.1%, cooling to 60-70 ℃, adding an ultraviolet absorbent, an antioxidant, a defoaming agent, a base material wetting agent and a catalyst, and stirring for 20-30min to obtain a component A;
(2) and B component: adding the polyether glycol with the formula amount into a reaction kettle, heating to 95-100 ℃, dehydrating under the condition of-0.1 MPa to enable the water content to reach 0.05%, then cooling to 50 ℃, adding the isocyanate with the formula amount, reacting for 2-2.5 hours at 80-85 ℃, cooling to 50 ℃, adding the latent curing agent with the formula amount, stirring for 20-30min, and barreling to obtain the component B.
(3) When in use, the A, B components are mixed uniformly according to the proportion to obtain the polyurethane caulking glue.
The invention reduces the product viscosity by selecting low molecular weight polyether and low viscosity plasticizer; by reasonably compounding polyether polyols with different molecular weights in the component A and the component B, microphase separation is facilitated, so that the mechanical property of the polyurethane caulking compound is improved; on the premise of ensuring low viscosity, the latent curing agent is selected to react with water (or moisture) preferentially to generate an active group, and then the active group and an isocyanate group are crosslinked and cured rapidly, so that the isocyanate and water are effectively prevented from reacting to generate gas, the foaming and bulging conditions are avoided, and the strength of the product is prevented from being reduced; the foaming rate is reduced by selecting a defoaming agent, and a micro-foaming or non-foaming product is obtained.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention solves the problems of easy cracking and poor caking property of the conventional product by selecting proper raw materials and auxiliary agents; the prepared product has low feed liquid viscosity, is easy to fill, can completely fill the gap space, does not foam, and ensures the product quality; the concrete has excellent physical properties such as tensile strength, elongation at break and the like, has good flexibility, meets the expansion change of a cement concrete foundation, and can be constructed in a certain humid environment;
(2) The operation time of the product prepared by the invention is 30-40min, the large-area construction of a field is convenient, and a good curing effect can be achieved within 6-8 h; in addition, the paint does not contain volatile substances, is safe and environment-friendly, and does not influence human bodies and the environment in the preparation, construction and use processes.
(3) The preparation method provided by the invention is simple in process and beneficial to industrial production.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
The percentages of the raw materials used in the following examples are by mass.
Example 1
the preparation method of the high-performance polyurethane caulking compound comprises the following steps:
(1) Preparing a component A: firstly, MN-305050%, 400-mesh talcum powder 20%, dioctyl phthalate 20% and MOCA 5% are put into a kettle and uniformly stirred, the temperature is increased to 85-90 ℃, dehydration is carried out under the condition of vacuum degree of-0.1 MPa, the water content is reduced to be below 0.1%, the temperature is reduced to 60-70 ℃, 1% of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 1% of 3, 5-di-tert-butyl-4-hydroxy-phenylpropionic acid isooctyl ester, 1% of BYK-A53561%, BYK-3071% and 1% of dibutyltin dilaurate are added and stirred for 20-30 minutes, and the component A is obtained;
(2) Preparing a component B: adding DL-300050% and DV 12520% into a reaction kettle, stirring and heating to 95-100 ℃, dehydrating under-0.1 MPa, using water content to be below 0.05%, then cooling to 50 ℃, adding MDI-5029%, reacting at 80-85 ℃ for 2-2.5 hours, cooling to 50 ℃, adding Incorez HP 1%, stirring for 20min, and barreling to obtain the component B.
(3) When in use, the A, B components are evenly mixed according to the mass ratio of 1:1 and then are spread.
Example 2
The preparation method of the high-performance polyurethane caulking compound comprises the following steps:
(1) preparing a component A: putting DL-40020%, DL-300023%, 400-mesh talcum powder 30%, dimethyl adipate 20% and DMTDA 3% into a kettle, uniformly stirring, heating to 85-90 ℃, dehydrating under the vacuum degree of-0.1 MPa to ensure that the water content is below 0.1%, cooling to 60-70 ℃, adding 0.7% of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 0.8% of 3, 5-di-tert-butyl-4-hydroxy-phenylpropionic acid isooctyl ester, BYK-A5061%, BYK-3441% and 0.5% of dibutyltin dilaurate, and stirring for 20-30 minutes to obtain a component A;
(2) Preparing a component B: adding MN-305044% and DL-200030% into a reaction kettle, stirring and heating to 95-100 ℃, dehydrating under the condition of-0.1 MPa, using water content to be less than 0.05%, then cooling to 50 ℃, adding MDI-10025%, reacting at 80-85 ℃ for 2-2.5 hours, cooling to 50 ℃, adding Incorez HP 1%, stirring for 20min, and barreling to obtain the component B.
(3) When in use, the A, B components are evenly mixed according to the mass ratio of 3:1 and then are spread.
example 3
The preparation method of the high-performance polyurethane caulking compound comprises the following steps:
(1) Preparing a component A: firstly, putting DL-300020%, DL-100020%, 400-mesh talcum powder 30%, dibutyl phthalate 24% and MOCA 3% into a kettle, uniformly stirring, heating to 85-90 ℃, dehydrating under the condition of vacuum degree of-0.1 MPa to ensure that the water content is below 0.1%, cooling to 60-70 ℃, adding 0.5% of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 0.5% of 3, 5-di-tert-butyl-4-hydroxy-phenylpropionic acid isooctyl ester, BYK-A5060.5%, BYK-3071% and 0.5% of dibutyltin dilaurate, and stirring for 20-30 minutes to obtain a component A;
(2) preparing a component B: adding DV 12530% and MN-305040% into a reaction kettle, stirring and heating to 95-100 ℃, dehydrating under the condition of-0.1 MPa, using water content to be below 0.05%, then cooling to 50 ℃, adding 29.5% of liquefied MDI, reacting at 80-85 ℃ for 2-2.5 hours, cooling to 50 ℃, adding 0.5% of Incorez HP, stirring for 20min, and barreling to obtain the component B.
(3) When in use, the A, B components are evenly mixed according to the mass ratio of 5:1 and then are spread.
The three groups of example products were tested for physical properties with a commercial caulk product, and the results are shown in table 1.
Table 1 performance data for products of examples 1-3 and market products
note: the yellowing resistance test method is that continuous irradiation is carried out in a xenon lamp aging box under the environment of 55 ℃.
"> 100 h" indicates that no yellowing occurred for more than 100 h.
As can be seen from the table above, compared with two market caulking compound products, the product of the embodiment has remarkable advantages in tensile strength, elongation at break, cohesiveness and yellowing resistance, the elastic recovery rate is also kept at a better level, the use effect is good in a humid environment, and the market demand can be better met.
Claims (10)
1. The high-performance polyurethane caulking glue comprises a component A and a component B, and is characterized in that: the mass ratio of the component A to the component B is 1-5:1, wherein,
The component A comprises the following raw materials in percentage by mass:
The component B comprises the following raw materials in percentage by mass:
Polyether polyol 60-80%
10-40% of isocyanate
0.5 to 2 percent of latent curing agent;
The polyether polyol has a functionality of 2-3 and a number average molecular weight of 300-4000.
2. the high performance polyurethane caulk according to claim 1, wherein: the polyether polyol is one or more of MN-3050, DL-3000, DL-1000, DL-400 or DV 125.
3. the high performance polyurethane caulk according to claim 1, wherein: the filler is one or two of 400-mesh talcum powder or 600-mesh talcum powder.
4. The high performance polyurethane caulk according to claim 1, wherein: the plasticizer is one or more of dibutyl phthalate, dioctyl phthalate or dimethyl adipate.
5. The high performance polyurethane caulk according to claim 1, wherein: the chain extender is one or two of MOCA and 3, 5-dimethylthio toluenediamine; the ultraviolet absorbent is 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole.
6. the high performance polyurethane caulk according to claim 1, wherein: the antioxidant is 3, 5-di-tert-butyl-4-hydroxy-phenylpropionic acid isooctyl ester; the catalyst was dibutyltin dilaurate.
7. The high performance polyurethane caulk according to claim 1, wherein: the defoaming agent is one or two of BYK-A506 or BYK-A5356.
8. The high performance polyurethane caulk according to claim 1, wherein: the base material wetting agent is BYK-307 or BYK-344; the latent curing agent was Incorez HP.
9. the high performance polyurethane caulk according to claim 1, wherein: the isocyanate is one or more of MDI-5, MDI-100 or liquefied MDI.
10. A method for preparing the high-performance polyurethane caulk according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) The component A comprises: firstly, putting polyether polyol, a filler, a plasticizer and a chain extender in a formula ratio into a kettle, uniformly stirring, heating to 85-90 ℃, dehydrating under the condition of vacuum degree of-0.1 MPa to ensure that the water content is below 0.1%, cooling to 60-70 ℃, adding an ultraviolet absorbent, an antioxidant, a defoaming agent, a base material wetting agent and a catalyst, and stirring for 20-30min to obtain a component A;
(2) And B component: adding polyether glycol with the formula amount into a reaction kettle, heating to 95-100 ℃, dehydrating under the condition of-0.1 MPa to enable the water content to reach 0.05%, then cooling to 50 ℃, adding isocyanate with the formula amount, reacting for 2-2.5 hours at 80-85 ℃, cooling to 50 ℃, adding latent curing agent with the formula amount, stirring for 20-30min, and barreling to obtain a component B;
(3) When in use, the A, B components are mixed uniformly according to the proportion to obtain the polyurethane caulking glue.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110885662A (en) * | 2019-12-16 | 2020-03-17 | 山东一诺威聚氨酯股份有限公司 | Pouring sealant for polyurethane soft-package battery and preparation method thereof |
| CN111777983A (en) * | 2020-06-23 | 2020-10-16 | 山东一诺威聚氨酯股份有限公司 | High-hardness heat-conducting polyurethane structural adhesive and preparation method thereof |
| CN112680088A (en) * | 2020-12-28 | 2021-04-20 | 山东一诺威聚氨酯股份有限公司 | Thick-coatable single-component polyurethane material and preparation method thereof |
| CN113737531A (en) * | 2021-09-26 | 2021-12-03 | 深圳市联星服装辅料有限公司 | Impregnation liquid, waterborne polyurethane impregnation polyester cord and preparation method thereof |
-
2019
- 2019-09-27 CN CN201910923726.5A patent/CN110551480A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110885662A (en) * | 2019-12-16 | 2020-03-17 | 山东一诺威聚氨酯股份有限公司 | Pouring sealant for polyurethane soft-package battery and preparation method thereof |
| CN111777983A (en) * | 2020-06-23 | 2020-10-16 | 山东一诺威聚氨酯股份有限公司 | High-hardness heat-conducting polyurethane structural adhesive and preparation method thereof |
| CN112680088A (en) * | 2020-12-28 | 2021-04-20 | 山东一诺威聚氨酯股份有限公司 | Thick-coatable single-component polyurethane material and preparation method thereof |
| CN113737531A (en) * | 2021-09-26 | 2021-12-03 | 深圳市联星服装辅料有限公司 | Impregnation liquid, waterborne polyurethane impregnation polyester cord and preparation method thereof |
| CN113737531B (en) * | 2021-09-26 | 2023-10-20 | 深圳市联星服装辅料有限公司 | Dipping liquid, aqueous polyurethane dipping polyester rope and preparation method thereof |
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Application publication date: 20191210 |