CN110951032A - Fast curing type silicon PU material and preparation method thereof - Google Patents
Fast curing type silicon PU material and preparation method thereof Download PDFInfo
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- 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
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
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- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
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- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
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- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
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Abstract
The invention belongs to the technical field of polyurethane, and particularly relates to a fast curing type silicon PU material and a preparation method thereof. The rapid curing type silicon PU material consists of a component A and a component B; the component A consists of polyether polyol, a filler, a plasticizer, a chain extender, a pigment, an ultraviolet absorber, an antioxidant, a catalyst, a defoaming agent and a thixotropic additive, the component B consists of polyether polyol, isocyanate and a storage stabilizer, and the mass ratio of the component A to the component B is 4-6: 1. The rapid curing type silicon PU material provided by the invention has the advantages that the curing speed of silicon PU is increased, the construction is convenient, the construction efficiency is improved, the wear resistance and flexibility are better, and the problem of long construction period of the traditional silicon PU material is effectively solved; the invention also provides a preparation method of the composition.
Description
Technical Field
The invention belongs to the technical field of polyurethane, and particularly relates to a fast curing type silicon PU material and a preparation method thereof.
Background
The silicon PU material is a new generation of court paving material developed and developed on the basis of the traditional PU court material. The composite material has good buffering property, ductility, wear resistance and the like, so that the composite material is widely applied to the construction of sports grounds such as basketball courts, badminton courts, tennis courts and the like. The silicon PU material effectively overcomes the defects of the PU court material in the aspects of professional performance, environment-friendly construction, service life, daily maintenance and the like, and has revolutionary innovation. However, the silicon PU has higher construction requirement, large viscosity of feed liquid and long curing time, and the next procedure construction can be carried out after the time of waiting for 24 hours generally, so that the construction difficulty is increased to a great extent, and the construction efficiency is reduced.
Although the existing polyurea material has the characteristics of fast curing, high strength, excellent aging resistance and corrosion resistance and the like, the curing speed is very fast, the gel is not sticky in less than one minute, professional spraying equipment is required for construction, the cost is high, the once spraying thickness is limited, the toughness of a finished product is poor, and the application range of a polyurea product is influenced; although the epoxy terrace also has higher curing speed and higher strength, the epoxy terrace has higher hardness and poor comfort, and is easy to crack along with a foundation, so that the service life is greatly reduced.
Therefore, a silicon PU product which has a short construction period, can be put into use quickly after completion, has high strength and elasticity, is low in VOC content, and is safe and environment-friendly is urgently needed in the market.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a fast curing type silicon PU material, which improves the curing speed of the silicon PU, is convenient to construct, improves the construction efficiency, has better wear resistance and flexibility, and effectively solves the problem of long construction period of the traditional silicon PU material; the invention also provides a preparation method of the composition.
The rapid curing type silicon PU material consists of a component A and a component B;
the component A comprises the following raw materials in percentage by mass:
the component B comprises the following raw materials in percentage by mass and 20ppm of storage stabilizer:
polyether polyol 60-70%
30-40% of isocyanate;
the mass ratio of the component A to the component B is 4-6: 1.
The polyether polyol is low-unsaturation high-activity polyether polyol with the functionality of 2-3 and the number average molecular weight of 300-2000. Preferably MN-500, MN-700 or DV125 (east Lanzhong).
The isocyanate is HDI biuret polyisocyanate, polymeric MDI or liquefied MDI.
The filler is 400 meshes of talcum powder.
The pigment is iron oxide green.
The plasticizer is one or more of dibutyl phthalate, dioctyl phthalate and dimethyl adipate.
The chain extender is XYLink 740M (Suzhou Xiangyuan New Material Co., Ltd.) or TDMA-02 (Guangzhou Youyun synthetic materials Co., Ltd.).
The external absorbent is 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole.
The antioxidant is 3, 5-di-tert-butyl-4-hydroxy-phenylpropionic acid isooctyl ester.
The catalyst is CUCAT-TM (Guangzhou Youyun synthetic materials Co., Ltd.).
The defoaming agent is organosilicon defoaming agent BYK-066N or BYK-024 (Germany BYK chemical company).
The thixotropic additive is a polyamide wax MT PLUS (Taurumette. TM. J. Co., Ltd.).
The storage stabilizer is phosphoric acid or benzoyl chloride.
The preparation method of the rapid curing type silicon PU material comprises the following steps:
(1) the component A comprises: firstly, polyether polyol, a filler, a pigment, a plasticizer, a chain extender and a thixotropic additive in a formula amount are mixed and stirred uniformly, the temperature is increased to 85-90 ℃, dehydration is carried out under the condition of vacuum degree of-0.1 MPa, the moisture content is reduced to below 0.1 percent, the temperature is reduced to 60-70 ℃, and then an ultraviolet absorbent, an antioxidant, a defoaming agent and a catalyst are added and stirred uniformly, so as to obtain a component A;
(2) and B component: heating polyether glycol in a formula amount to 95-100 ℃, dehydrating under the condition of-0.1 MPa to enable the water content to be below 0.05%, then cooling to 50-60 ℃, adding isocyanate in a formula amount, reacting for 2-2.5h at 80-85 ℃, cooling to 50-60 ℃, adding a storage stabilizer in a formula amount, and uniformly stirring to obtain a component B;
(3) when in use, the A, B components are evenly mixed and spread, and the fast curing type silicon PU material is obtained after curing.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, polyether polyol and isocyanate which have relatively high reaction speed are matched, so that the curing speed is improved, and excellent strength can be achieved after construction for 4-6 h; the proper catalyst is added cooperatively, so that the flow time of the A, B mixed component is improved and prolonged emphatically, sufficient operable time is ensured during construction, and the problems of long curing time and poor operability of conventional products are solved;
(2) according to the invention, the polyamide wax is uniformly dispersed in the whole system and forms intermolecular hydrogen bonds, when the intermolecular hydrogen bonds are subjected to shearing force, the molecular adhesion is pulled, the structure is damaged, the viscosity is reduced, and the problem of high viscosity of the feed liquid in the silicon PU construction process is solved;
(3) the product of the invention does not contain MOCA and volatile substances, is safe and environment-friendly, does not affect human bodies and environment in the preparation, construction and use processes, and has simple preparation method, simple process and convenient production.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited thereto, and modifications of the technical solutions of the present invention by those skilled in the art should be within the scope of the present invention.
The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature.
Example 1
Preparing a component material A: firstly, 70050 percent of MN, 30 percent of 400-mesh talcum powder, 0.5 percent of iron oxide green, 10 percent of dioctyl phthalate, 740M 5 percent of XYlink and 1 percent of MT PLUS are put into a kettle and uniformly stirred, the temperature is increased to 85 ℃, the dehydration is carried out under the condition of vacuum degree of-0.1 MPa, the moisture content reaches below 0.1 percent, the temperature is reduced to 60 ℃, 1 percent of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 1 percent of 3, 5-di-tert-butyl-4-hydroxy-iso-octyl phenylpropionate, 1 percent of CUCAT-TM and 0.5 percent of BYK-066N are added and stirred for 20 minutes, and a component A product is obtained;
preparing a component B material: adding DL-100065% into a reaction kettle, stirring and heating to 95 ℃, dehydrating under the condition of-0.1 MPa, reducing the water content to be below 0.05%, then cooling to 50 ℃, adding M20S 35% to react for 2 hours at 85 ℃, cooling to 50 ℃, adding 20ppm of phosphoric acid, stirring for 20min, and barreling to obtain a component B product;
when in use, the A, B components are evenly mixed according to the mass ratio of 5:1 and then are spread.
Example 2
Preparing a component material A: putting DV 12540%, 400-mesh talcum powder 32%, iron oxide green 1%, dimethyl adipate 20%, TDMA-023% and MT PLUS 1% into a kettle, uniformly stirring, heating to 85 ℃, dehydrating under the condition of vacuum degree of-0.1 MPa to enable the water content to reach below 0.1%, cooling to 70 ℃, adding 0.7% of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 0.8% of 3, 5-di-tert-butyl-4-hydroxy-iso-octyl phenylpropionate, BYK-0241% and CUCAT-TM 0.5%, stirring for 20 minutes to obtain a component A product;
preparing a component B material: adding DL-200060% into a reaction kettle, stirring and heating to 95 ℃, dehydrating under the condition of-0.1 MPa, and enabling the water content to be below 0.05%. Then cooling to 50 ℃, adding 40% of liquefied MDI, reacting for 2.5 hours at 80 ℃, cooling to 50 ℃, adding 20ppm of phosphoric acid, stirring for 20min, and barreling to obtain a component B product;
when in use, the A, B components are evenly mixed according to the mass ratio of 6:1 and then are spread.
Example 3
Preparing a component material A: firstly, MN-50032%, 400-mesh talcum powder 40%, iron oxide green 1%, dibutyl phthalate 20%, XYLink 740M 4% and MT PLUS 0.5% are put into a kettle and stirred uniformly, the temperature is increased to 90 ℃, the 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 ℃, 0.5% of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 0.5% of 3, 5-di-tert-butyl-4-hydroxy-iso-octyl phenylpropionate, BYK-0240.8% and CUCAT 0.7% are added and stirred for 30 minutes, and a component A product is obtained;
preparing a component B material: adding DL-200070% into a reaction kettle, stirring and heating to 100 ℃, dehydrating under the condition of-0.1 MPa, and enabling the water content to be below 0.05%. Then cooling to 50 ℃, adding HDI biuret polyisocyanate 30%, reacting for 2 hours at 85 ℃, cooling to 50 ℃, adding benzoyl chloride 20ppm, stirring for 20min, and barreling to obtain a component B product;
when in use, the A, B components are evenly mixed according to the mass ratio of 4:1 and then are spread.
Comparative example 1
Preparing a component material A: putting EP-330N 36%, 400-mesh talcum powder 35%, iron oxide green 1%, dimethyl adipate 20% and TDMA-025% into a kettle, uniformly stirring, heating to 85 ℃, dehydrating under the vacuum degree of-0.1 MPa to ensure that the water content is below 0.1%, cooling to 70 ℃, adding 0.7% of 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole, 0.8% of 3, 5-di-tert-butyl-4-hydroxy-iso-octyl phenylpropionate, 0.5% of BYK-0241% and 0.5% of organic bismuth catalyst, and stirring for 20 minutes to obtain a component A product;
preparing a component B material: adding DL-200062% into a reaction kettle, stirring and heating to 95 ℃, dehydrating under the condition of-0.1 MPa, and enabling the water content to be below 0.05%. Then cooling to 50 ℃, adding MDI-5038 percent, reacting for 2 hours at 80 ℃, cooling to 50 ℃, adding 20ppm phosphoric acid, stirring for 20min, and barreling to obtain a component B product;
when in use, the A, B components are evenly mixed according to the mass ratio of 5:1 and then are spread.
Comparative example 2
Commercially available polyurea products.
Comparative example 3
Commercial epoxy floor products.
The products of examples 1-3 and comparative examples 1-3 and market products are tested for physical properties according to standards, wherein a Shore D hardness tester is selected for testing the polyurea and epoxy terrace due to relatively high hardness, and the testing method comprises the following steps:
(1) shore hardness test is referred to GB/T531.1;
(2) the tensile strength and elongation at break tests are referred to GB/T10654.
The test results are shown in table 1.
TABLE 1 product Performance test data for examples 1-3 and comparative examples 1-3
As can be seen from Table 1, the silicon PU product prepared by the invention has moderate working life, short curing time, better product hardness, tensile strength and elongation at break, and can better meet the market demand. Comparative example 1 compared with the examples, the polyether polyol and the catalyst species were changed, and the thixotropic additive was not contained, the curing time and tensile properties of the article were significantly different, and the field workability was not good. The commercial polyurea product of comparative example 2 has the characteristics of fast curing and high strength, but has extremely fast curing speed and short operation time, requires professional spraying equipment for construction, and has poor toughness of the finished product, compared with the examples. Compared with the examples, the commercial epoxy floor product of the comparative example 3 has higher curing speed and higher strength, but has higher hardness, poorer toughness, poor comfort, easy cracking along with the foundation and shorter service life.
Claims (10)
1. A fast curing type silicon PU material is characterized in that: consists of a component A and a component B;
the component A comprises the following raw materials in percentage by mass:
the component B comprises the following raw materials in percentage by mass and 20ppm of storage stabilizer:
polyether polyol 60-70%
30-40% of isocyanate;
the mass ratio of the component A to the component B is 4-6: 1.
2. The fast-curing silicon PU material of claim 1, wherein: the polyether polyol is low-unsaturation high-activity polyether polyol with the functionality of 2-3 and the number average molecular weight of 300-2000.
3. The fast-curing silicon PU material of claim 1, wherein: the isocyanate is HDI biuret polyisocyanate, polymeric MDI or liquefied MDI.
4. The fast-curing silicon PU material of claim 1, wherein: the filler is 400 meshes of talcum powder, and the pigment is iron oxide green.
5. The fast-curing silicon PU material of claim 1, wherein: the plasticizer is one or more of dibutyl phthalate, dioctyl phthalate and dimethyl adipate.
6. The fast-curing silicon PU material of claim 1, wherein: the chain extender is XYlink 740M or TDMA-02.
7. The fast-curing silicon PU material of claim 1, wherein: the ultraviolet absorbent is 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-butylphenyl) benzotriazole; the antioxidant is 3, 5-di-tert-butyl-4-hydroxy-phenylpropionic acid isooctyl ester; the catalyst is CUCAT-TM; the defoaming agent is an organic silicon defoaming agent BYK-066N or BYK-024.
8. The fast-curing silicon PU material of claim 1, wherein: the thixotropic additive is polyamide wax MT PLUS.
9. The fast-curing silicon PU material of claim 1, wherein: the storage stabilizer is phosphoric acid or benzoyl chloride.
10. A method for preparing a fast-curing silicon PU material according to any one of claims 1 to 9, characterized in that: the method comprises the following steps:
(1) the component A comprises: firstly, polyether polyol, a filler, a pigment, a plasticizer, a chain extender and a thixotropic additive in a formula amount are mixed and stirred uniformly, the temperature is increased to 85-90 ℃, dehydration is carried out under the condition of vacuum degree of-0.1 MPa, the moisture content is reduced to below 0.1 percent, the temperature is reduced to 60-70 ℃, and then an ultraviolet absorbent, an antioxidant, a defoaming agent and a catalyst are added and stirred uniformly, so as to obtain a component A;
(2) and B component: heating polyether glycol in a formula amount to 95-100 ℃, dehydrating under the condition of-0.1 MPa to enable the water content to be below 0.05%, then cooling to 50-60 ℃, adding isocyanate in a formula amount, reacting for 2-2.5h at 80-85 ℃, cooling to 50-60 ℃, adding a storage stabilizer in a formula amount, and uniformly stirring to obtain a component B;
(3) when in use, the A, B components are evenly mixed and spread, and the fast curing type silicon PU material is obtained after curing.
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Cited By (6)
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| 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 |
| CN112877024A (en) * | 2021-02-04 | 2021-06-01 | 上海都昱新材料科技有限公司 | Anti-sagging polyurethane adhesive and preparation method and application thereof |
| CN113026478A (en) * | 2021-02-08 | 2021-06-25 | 山东世纪联合新材料科技有限公司 | High-elastic composite silicon PU court surface layer and construction method thereof |
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2019
- 2019-12-18 CN CN201911309880.XA patent/CN110951032A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112877024A (en) * | 2021-02-04 | 2021-06-01 | 上海都昱新材料科技有限公司 | Anti-sagging polyurethane adhesive and preparation method and application thereof |
| CN113026478A (en) * | 2021-02-08 | 2021-06-25 | 山东世纪联合新材料科技有限公司 | High-elastic composite silicon PU court surface layer and construction method thereof |
| WO2023226133A1 (en) * | 2022-05-24 | 2023-11-30 | 广东汇齐新材料有限公司 | Ultralow-hardness low-temperature activated thermoplastic polyurethane hot melt adhesive film and preparation method therefor |
| CN115011101A (en) * | 2022-07-14 | 2022-09-06 | 江苏长诺运动场地新材料有限公司 | High-suspension double-component polyurethane slurry and preparation method thereof |
| CN115011101B (en) * | 2022-07-14 | 2023-11-21 | 江苏长诺运动场地新材料有限公司 | High-suspension-property double-component polyurethane slurry and preparation method thereof |
| CN115466592A (en) * | 2022-11-02 | 2022-12-13 | 山东一诺威聚氨酯股份有限公司 | High-weather-resistance non-yellowing adhesive and preparation method thereof |
| CN115466592B (en) * | 2022-11-02 | 2023-03-24 | 山东一诺威聚氨酯股份有限公司 | High-weather-resistance non-yellowing adhesive and preparation method thereof |
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Application publication date: 20200403 |