CN108610934B - Single-component polyurethane waterproof coating, preparation method thereof and composition for preparing single-component polyurethane waterproof coating - Google Patents
Single-component polyurethane waterproof coating, preparation method thereof and composition for preparing single-component polyurethane waterproof coating Download PDFInfo
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Abstract
The invention relates to a composition for preparing a one-component polyurethane waterproof coating, which comprises the following components in percentage by weight: talcum powder or light calcium powder or a mixture of the talcum powder and the light calcium powder which are treated together with a rare earth coupling agent. The invention also relates to a novel environment-friendly single-component polyurethane waterproof coating containing the composition and a preparation method thereof. The method comprises (1) treating the mixture of talcum powder and light calcium carbonate powder with rare earth coupling agent to obtain material A; (2) fully reacting polyether polyol with diphenylmethane diisocyanate under certain conditions to obtain a material B; (3) mixing the material A and the material B together with an organic bismuth catalyst and other additives in proportion at a temperature of 60-80 ℃ to obtain the single-component polyurethane waterproof coating. The polyurethane waterproof coating provided by the invention is an environment-friendly single-component environment-friendly solvent-free polyurethane waterproof material. The polyurethane waterproof coating is non-toxic and tasteless, does not contain a solvent, TDI, a toxic catalyst, MOCA and other suspected carcinogens, is easy to obtain auxiliary materials, and has viscosity within a very ideal range, so that the field construction is convenient and rapid, and the curing speed of the winter construction is adjustable.
Description
Technical Field
The invention relates to the field of polyurethane waterproof coatings. In particular, the invention relates to a one-component polyurethane waterproof coating, a method for preparing the one-component polyurethane waterproof coating and a composition for preparing the one-component polyurethane waterproof coating.
Background
The green chemistry proposal makes us look into the good future of human beings. Green chemistry is also known as environmentally benign chemistry, environmentally friendly chemistry, clean chemistry, and the corresponding technology is also known as green technology. The corresponding product is also called green product. In China, the development direction of the construction chemical industry is as follows: water-based, high solid differentiation and non-toxic. Regardless of how toxic a substance is, it must only enter the body to function, which is known as bioavailability. The less bioavailable, the less harmful. Although people also find effective solutions for the pollution problem of chemical products, in order to thoroughly solve the harm of chemicals to human health and human living environment, a green chemical product, which is a substitute of toxic chemicals, needs to be continuously manufactured.
Waterproof materials, as a large class of building chemicals, certainly should exert their own desired effects in the greening and non-toxic conversion of products. In view of the present situation, although various new waterproof materials are emerging, most of them are far from greening.
Polyurethane waterproofing coatings are a potential green chemical product. The polyurethane waterproof coating has about forty years of application history in China, so that the polyurethane waterproof coating becomes a mature technology in the aspects of production, design, construction and the like. The 'nine-five' plan, the outline of the 2010 development plan and the 'fifteen' plan of the national chemical building materials list the polyurethane waterproof coating as a waterproof coating variety with key development, and the national building material industry standard JC/T500-92 polyurethane waterproof coating and the national standard GB/T19250-2003 polyurethane waterproof coating are issued in sequence. GB/T19250-2013 polyurethane waterproof coating and JC1066-2008 harmful substance limit in building waterproof coating.
At present, polyurethane waterproof materials on the market are divided into single-component polyurethane waterproof materials and double-component polyurethane waterproof materials. Compared with the two-component polyurethane waterproof coating, the single-component polyurethane waterproof coating saves the batching process before construction when in use, does not need metering and proportioning, and is convenient to use and operate; the coating film has smooth surface and no bubbles or pinholes; the application time is long. Therefore, the single-component polyurethane waterproof material has obvious advantages in material use compared with the two-component polyurethane waterproof material.
Regardless of whether the single-component polyurethane waterproof material or the two-component polyurethane waterproof material is adopted, the components in the traditional formula are all composed of polyether, Toluene Diisocyanate (TDI), a plasticizer, a solvent, a catalyst, a pigment and filler, an amine or alcohol curing agent and other auxiliaries. Wherein the Toluene Diisocyanate (TDI) is colorless liquid with strong pungent smell, boiling point is 251 deg.C, specific gravity is 1.22, and it turns black when exposed to light. Since TDI has high vapor pressure, TDI has strong smell and toxicity. In addition, the single-component polyurethane waterproof material containing TDI has extremely long surface drying time during winter construction, and certainly has extremely long actual drying time, so that the construction period in winter is too long. While the vapor pressure of diphenylmethane-methane-diisocyanate (MDI) at 160 ℃ is only 0.8mmHg (TDI reaches 10mmHg at 120 ℃, and 1mmHg is 133.322Pa), and the volatility in the production and use process is extremely low. In addition, MOCA has been highly suspected to have carcinogenic effects as a crosslinker for polyurethane waterproofing coatings. Accordingly, the one-pack type polyurethane waterproofing paint based on MDI using water as a crosslinking agent has been increasingly considered in consideration of the requirement of green products.
In addition, organotin and organolead catalysts contained in the polyurethane waterproof materials in the current market have high toxicity, and the content of the organotin and organolead catalysts in some formulas is also high. Recently developed organobismuth catalysts have been greatly developed in view of the requirement for green products.
However, in general, for one-pack polyurethane waterproofing paints which do not contain a solvent and use MDI which is more environmentally friendly than TDI, the viscosity of the material is large and the open time is still long, which makes the workability of the material in winter impossible to be secured, thereby greatly limiting the application of such a preferred waterproofing paint.
Disclosure of Invention
Based on the problems in the prior art as described above, there is a need for a one-component polyurethane waterproof coating material, a method for preparing the one-component polyurethane waterproof coating material, and a composition for preparing the one-component polyurethane waterproof coating material.
According to one aspect of the invention, a preparation method of a one-component polyurethane waterproof coating is provided, which comprises the following steps:
(1) fully activating a 1: 1 mixture of 600-mesh talcum powder and 400-mesh light calcium carbonate with a rare earth coupling agent at 72 +/-2 ℃ to obtain a material A;
(2) fully polymerizing polyether polyol and diphenylmethane diisocyanate according to an equivalent ratio of 1: 2.05 under a preset condition to obtain a material B;
(3) mixing the material A and the material B according to the weight ratio of 1: 1 with an organic bismuth catalyst and an additive at the temperature of 60-80 ℃ for 3-4 hours to obtain the single-component polyurethane waterproof coating.
In one embodiment, the organobismuth catalyst is BICAT8118 with a bismuth content of 18%.
In one embodiment, the diphenylmethane diisocyanate is a mixture of 4, 4 '-diphenylmethane diisocyanate and 2, 4' -diphenylmethane diisocyanate.
In one embodiment, the molar ratio of 4, 4 '-diphenylmethane diisocyanate to 2, 4' -diphenylmethane diisocyanate is 1: 1, 1: 2, or 2: 1.
In one embodiment, the polyether polyol comprises a mixture of a low unsaturation polyether diol having a molecular weight of 1000-.
In one embodiment, the mass ratio of the low unsaturation polyether diol to the low unsaturation polyether triol is 4: 1;
the unsaturation degree of the low unsaturation degree polyether dihydric alcohol and the low unsaturation degree polyether trihydric alcohol is not more than 0.007 mol/kg.
In one embodiment, the additive comprises one or more of a gas absorber, a pigment, an antioxidant, an ultraviolet absorber.
According to another aspect of the present invention, there is also provided a composition for preparing a one-component polyurethane waterproof coating material, the composition comprising: talc powder, light calcium carbonate or a mixture of the two, treated with a rare earth coupling agent; wherein the mass ratio of the talcum powder to the light calcium carbonate is 1: 1.
According to another aspect of the invention, a one-component polyurethane waterproof coating is also provided, and the waterproof coating comprises the composition.
According to another aspect of the present invention, there is also provided a one-component polyurethane waterproof coating material prepared by the method according to any one of the above.
The single-component polyurethane waterproof coating prepared by the invention is cured into a film through reaction with moisture in the air, namely, water is used as a cross-linking agent, urea bonds are introduced, so that the material performance is improved, MOCA (metal organic aluminum) used as a pollution source is abandoned, and the green environmental-protection performance of the material is greatly improved by adopting an organic bismuth catalyst.
The polyurethane waterproof coating provided by the invention is an environment-friendly single-component environment-friendly solvent-free polyurethane waterproof material. The single-component polyurethane waterproof coating is non-toxic and tasteless, does not contain a solvent, TDI, a toxic catalyst, MOCA and other suspected carcinogens, is easy to obtain auxiliary materials, and can be conveniently and quickly constructed on site and adjustable in solidification speed in winter by activating powder in a system to ensure that the viscosity of the single-component polyurethane waterproof coating can be in a very ideal range.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
In order to solve the technical problems, the invention provides a method for preparing a one-component polyurethane waterproof coating.
A preparation method of a single-component polyurethane waterproof coating comprises the following steps:
(1) stirring 600-mesh talcum powder or 400-mesh light calcium carbonate or a mixture of the two in a ratio of 1: 1 with a rare earth coupling agent at 75 ℃ until the mixture is uniform to obtain a material A.
The talc of the present invention was commercially available 600 mesh talc and the precipitated calcium carbonate of the present invention was commercially available 400 mesh precipitated calcium carbonate. The particle size and the proportion are related to the viscosity, the cost and the storage stability of the prepared single-component polyurethane waterproof coating. The mixture of the mesh talcum powder and the mesh light calcium carbonate is used, and the ratio of the mixture is 1: 1.
The chemical general formula of the rare earth coupling agent is (C3H7O) xRe (OCOR') m (OCOR2) n (OAB) y. The substance is white or light yellow small granule solid, and has the characteristics of light color, no odor and no toxicity.
(2) Fully synthesizing polyether glycol and diphenylmethane diisocyanate according to an equivalent ratio of 1: 2.05 under certain conditions to obtain a material B;
(3) mixing the material A and the material B together with an organic bismuth catalyst and other selected additives according to the ratio of 1: 1 at the temperature of 60-80 ℃ for 3-4 hours to obtain the single-component polyurethane waterproof coating.
Wherein the organic bismuth catalyst adopts BICAT8118, wherein the bismuth content is 18 percent.
In one embodiment, the diphenylmethane diisocyanate is a mixture comprising 4, 4 '-diphenylmethane diisocyanate and 2, 4' -diphenylmethane diisocyanate.
In one embodiment, the weight ratio of 4, 4 '-diphenylmethane diisocyanate to 2, 4' -diphenylmethane diisocyanate is 1: 1, 1: 2 or 2: 1.
In one embodiment, the polyether polyol comprises a mixture of a low unsaturation polyether diol having a molecular weight of 1000 to 2000 and a low unsaturation polyether triol having a molecular weight of 3000 to 5000.
Wherein the mass ratio of the low-unsaturation polyether diol to the low-unsaturation polyether triol is 4: 1. The unsaturation degree of the low unsaturation degree polyether dihydric alcohol and the low unsaturation degree polyether trihydric alcohol is not more than 0.007 mol/kg.
In one embodiment, wherein the above additives comprise one or more of a gas absorber, a pigment, an antioxidant, an ultraviolet absorber. The addition can be selected according to the specific requirements of customers. For example, the apparent color (e.g., red or green) of the one-component polyurethane waterproofing paint is customized for the customer's choice. Still other users require that the construction be carried out at a specific site (under severe environmental conditions), and at this time, an antioxidant and an ultraviolet absorber should be added.
The gas absorbent used in the process of the present invention comprises fumed silica.
Pigments useful in the method of the present invention include carbon black, iron red and chromium green.
The antioxidant used in the method of the present invention includes antioxidant 1010.
The ultraviolet absorber used in the method of the present invention includes UV 327.
The environmentally friendly plasticizer used in the process of the present invention comprises tributyl citrate.
In another aspect, the present invention provides a one-component polyurethane waterproof coating material prepared by the method of the present invention as described above.
In another aspect, the present invention provides a composition for preparing a one-pack polyurethane waterproof coating material, the composition comprising: talc powder or light calcium carbonate or their mixture treated with rare earth coupling agent.
In another aspect, the present invention provides a one-component polyurethane waterproof coating comprising the composition of the present invention as described above.
The technical effects are achieved:
1) the composition is used in the method for preparing the one-component polyurethane waterproof coating, and the viscosity of the waterproof coating can be controlled at will by using the composition, so that the waterproof coating can have wider production and construction applicability as required.
2) The surface drying time of the single-component polyurethane waterproof material can be greatly adjusted in a wide range according to the proportion of MDI, so that the single-component polyurethane waterproof material can be easily constructed even in winter, and the production process and the construction period progress of the construction process are greatly improved and controlled; meanwhile, the storage period of the material completely reaches the standard.
3) The method of the invention uses diphenylmethane diisocyanate (MDI) and abandons poisonous and harmful TDI and solvent, thereby greatly improving and controlling the environmental pollution in the production process and the construction process.
4) The waterproof material has excellent performance indexes. The tensile strength, the elongation at break and the performance in construction in severe environment are excellent. Completely reaches the standards of GB/T19250 plus 2013 polyurethane waterproof paint and JC1066-2008 harmful substance limit in building waterproof paint. The formula does not contain any toxic substance.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail by examples below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following description will be given with reference to specific examples.
The parts in the following examples are parts by mass.
Example 1
Adding the mixture of talcum powder and light calcium in equal proportion into a reaction kettle, and heating to 74 ℃. And C, chopping the rare earth coupling agent under the stirring state, slowly adding the chopped rare earth coupling agent into the stirring reaction kettle, and fully and uniformly stirring to obtain the material A.
Polyether diol and polyether triol are mixed in the weight ratio of 4 to 1, vacuum dewatered at 100-120 deg.c for 3 hr, cooled to room temperature, and mixed with diphenyl methane diisocyanate MDI in the equivalent ratio of 1 to 2.05. Thus, material B was obtained. In this example, the diphenylmethane diisocyanate was a mixture of 4, 4 '-diphenylmethane diisocyanate and 2, 4' -diphenylmethane diisocyanate in a weight ratio of 1: 1. After stirring, the temperature is raised and kept at 80 ℃ for 3 hours. Then adding the material A according to the amount (the ratio of A to B is 1: 1), and continuously preserving the heat for 1 hour; then cooling to 60 ℃, adding quantitative additives (environment-friendly plasticizer and the like) and organic bismuth catalyst and the like, stirring uniformly, defoaming in vacuum and discharging. The environment-friendly single-component polyurethane waterproof material is obtained.
Various environmental protection indexes of final polyurethane waterproof coating
Wherein, the table shows the detection of the sample of the invention for the environmental and health related product safety of the Chinese disease prevention and control center. The detection method adopts 'Standard test method for Drinking Water' GB/T5750-2006; the sample treatment method is carried out according to the evaluation standard of sanitary safety of drinking water delivery and distribution equipment and protective materials. The samples were prepared as in section A13.1 of the appendix, with a soaking time of 24 hours and a soaking temperature of 25. + -. 5 ℃. The inspection result shows that indexes of color, turbidity, odor and taste, visible substances to the naked eyes, ph, total soluble solids, oxygen consumption, arsenic, cadmium, chromium (hexavalent), aluminum, lead, mercury, trichloromethane, volatile phenols, carbon tetrachloride, formaldehyde, epoxy chloropropane, styrene, benzene, toluene and xylene in the soaking water all meet the sanitary requirements of sanitary safety evaluation standards of domestic drinking water transmission and distribution equipment and protective materials on the protective materials. Therefore, the polyurethane waterproof coating is green, environment-friendly and sanitary.
Example 2
The difference between the example and the example 1 is that the ratio of 4, 4 '-MDI and 2, 4' -MDI is 2: 1, the mixture of talcum powder and light calcium is added into the reaction kettle to react at 72 ℃, the reaction temperature of the material A and the material B, the organic bismuth catalyst and the additive are 70 ℃ according to the weight ratio of 1: 1, the reaction temperature of the material A and the material B, the organic bismuth catalyst and the additive are 75 ℃ according to the weight ratio of 1: 1, and the rest is unchanged (the equivalent ratio of polyether polyol to diphenylmethane diisocyanate is 1: 2.05, and the ratio of the material A to the material B is 1: 1).
Example 3
This example differs from example 1 in that the ratio of 4, 4 '-MDI to 2, 4' -MDI was 1: 2, the reaction temperature of the talc and light calcium mixture added to the reactor was 70 ℃ and the rest was unchanged (polyether polyol to diphenylmethane diisocyanate in an equivalent ratio of 1: 2.05, and the ratio of material A to material B was 1: 1).
The corresponding modifications of 4, 4 '-MDI and 2, 4' -MDI in examples 1 to 3 above have the following effect on the properties of the coating:
effect of the 4, 4 '-MDI and 2, 4' -MDI mixture ratio on the Properties of the coatings
| 4.4’ MDI/2.4’ MDI | Tensile strength/MPa | Elongation at break/% | Viscosity/centipoise |
| 2∶1 | 2.84 | 800 | 18000 |
| 1∶2 | 2.08 | 540 | 7600 |
| 1∶1 | 2.62 | 750 | 13000 |
The indexes of the final polyurethane waterproof coating prepared by the three examples, such as tensile strength, elongation at break, viscosity range, surface drying time and the like, are as follows:
as can be seen from the above table, by adjusting the weight ratio of 4, 4 '-MDI and 2, 4' -MDI, the viscosity of the waterproof coating can be controlled, and various physical properties of the waterproof coating can reach the standard. In addition, the surface drying time of the waterproof material can be greatly adjusted in a wide range along with the change of the proportion of MDI, and the storage period reaches the standard.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. A preparation method of a single-component polyurethane waterproof coating comprises the following steps:
(1) fully activating a mixture of 600-mesh talcum powder and 400-mesh light calcium carbonate in a ratio of 1: 1 with a rare earth coupling agent at 72 +/-2 ℃ to obtain a material A;
(2) fully polymerizing polyether polyol and diphenylmethane diisocyanate according to an equivalent ratio of 1: 2.05 under a preset condition to obtain a material B;
(3) mixing the material A and the material B according to the weight ratio of 1: 1 with an organic bismuth catalyst and an additive at the temperature of 60-80 ℃ for 3-4 hours to obtain the single-component polyurethane waterproof coating;
wherein the polyether polyol comprises a mixture of low unsaturation polyether diol with molecular weight of 1000-2000-plus and low unsaturation polyether triol with molecular weight of 3000-5000-plus;
the diphenylmethane diisocyanate is a mixture of 4, 4 '-diphenylmethane diisocyanate and 2, 4' -diphenylmethane diisocyanate;
the molar ratio of the 4, 4 '-diphenylmethane diisocyanate to the 2, 4' -diphenylmethane diisocyanate is 1: 1 or 2: 1.
2. The method of claim 1 wherein the organobismuth catalyst is BICAT8118 with a bismuth content of 18%.
3. The method of claim 1, wherein the mass ratio of the low unsaturation polyether diol to the low unsaturation polyether triol is 4: 1.
4. The method of claim 1, wherein the additive comprises one or more of a gas absorber, a pigment, an antioxidant, and an ultraviolet absorber.
5. A one-component polyurethane waterproof paint characterized in that it is prepared by the method according to any one of claims 1 to 4.
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| CN111876061A (en) * | 2020-07-31 | 2020-11-03 | 潍坊市璇宝防水材料有限公司 | High-performance polyurethane waterproof coating and preparation method thereof |
| CN116285638B (en) * | 2022-12-23 | 2024-06-21 | 北京东方雨虹防水技术股份有限公司 | Drinking water-level solvent-free single-component polyurethane waterproof coating and preparation method thereof |
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| CN102181225A (en) * | 2011-01-31 | 2011-09-14 | 北京东方雨虹防水技术股份有限公司 | Water-cured polyurethane waterproof coating |
| CN104194610A (en) * | 2014-09-11 | 2014-12-10 | 北京东方雨虹防水技术股份有限公司 | Self-crosslinked one-component polyurethane waterproofing coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181225A (en) * | 2011-01-31 | 2011-09-14 | 北京东方雨虹防水技术股份有限公司 | Water-cured polyurethane waterproof coating |
| CN104194610A (en) * | 2014-09-11 | 2014-12-10 | 北京东方雨虹防水技术股份有限公司 | Self-crosslinked one-component polyurethane waterproofing coating |
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