CN114350243B - Single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material - Google Patents
Single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material Download PDFInfo
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Abstract
The invention discloses a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material, which comprises the following steps: preparing hydroxyl-terminated polyether prepolymer, synthesizing polyether, synthesizing polyurethane resin, and preparing single-liquid anti-sagging non-expansion waterproof thermal-insulation polyurethane material. The waterproof performance of the polyurethane waterproof coating is superior to that of polyurethane waterproof coating on the market, the polyurethane waterproof coating can have heat preservation performance under the condition of no foaming, and the heat conductivity coefficient is low due to the fact that fumed silica is used in a large amount in the material, and the polyurethane waterproof coating can be waterproof and heat preservation at the same time; the invention has high breaking elongation and high breaking strength between the epoxy and the polyurea, and can be used as an anti-cracking buffer layer in concrete protection to well solve the problem of zero extension; the invention can reduce the construction cost and reduce the construction steps.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material.
Background
In the aquaculture industry, concrete cracking is a common phenomenon because the base material of most aquaculture ponds is concrete. Meanwhile, because the aquaculture needs a constant-temperature environment, all the requirements for heat preservation of the aquaculture pond are also put forward. Compared with other materials, the polyurethane material has congenital advantages in strength, tensile strength and aging resistance, but the polyurethane material can keep warm but cannot resist water under the condition of foaming, and can resist water but cannot play a role in heat preservation under the condition of film forming. The prior art is as follows: 1. foaming polyurethane on concrete, and then making waterproof polyurethane on the foamed polyurethane. 2. And (3) independently painting epoxy paint. However, once the concrete base material cracks, surface water can be prevented from penetrating into the foaming polyurethane, and the porous foaming polyurethane provides a warm bed for a plurality of disease bacteria, but is difficult to kill, so that a great hidden danger is buried for subsequent cultivation.
Disclosure of Invention
The invention aims to provide a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material aiming at the defects and the shortcomings of the prior art.
In order to achieve the above purpose, the invention adopts the following technical scheme: the single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material is characterized by comprising the following technical steps:
s1, preparing hydroxyl-terminated polyether prepolymer: adding 210 g-250 g of citric acid monohydrate, 580 g-640 g of tripropylene glycol, 500 g-600 g of dimethylbenzene and 10 g-15 g of 98% concentrated sulfuric acid into a 2L flask, stirring, heating to reflux, and separating water by a water separator; stopping heating when the water separated from the water separator is 72 ml-80 ml; cooling to below 60 ℃ in air, adding 400ml of water, stirring for 5 minutes, pouring into a separating funnel, standing, discharging lower-layer liquid, adding water, and washing until the PH is greater than 6.5 to obtain an intermediate I;
s2, synthesizing polyether: adding 400-450 g of dimethylbenzene into a 5L flask, stirring, adjusting the rotating speed to 70-90 r/min, heating to reflux, separating water by a water separator until the methylbenzene in the water separator is clarified and cooled, introducing nitrogen for protection, and adding 860-900 g of 9 (ethoxy) trimethylolpropane to adjust the rotating speed to 90-120 r/min to obtain an intermediate II;
s3, synthesizing polyurethane resin: adding 0.8g of dibutyltin dilaurate and 10-15 g of latent curing agent into an intermediate II, heating to 65-85 ℃, dropwise adding 330-350 g of MDI (diphenylmethane diisocyanate), heating to reflux after the dropwise adding is completed, preserving heat for 2 hours, detecting the-NCO% in the mixture, and stopping the reaction when the-NCO% is 3.2-3.8%, thus obtaining resin I;
s4, manufacturing a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material: pouring the obtained resin I into a 10L high-speed stirrer to regulate the rotation speed to 150-200 r/min, preserving heat at 40-50 ℃, sequentially adding 60-80 g of acetyl tributyl citrate, 15-18 g of polyacrylamide, 100-250 g of titanium pigment, 500-550 g of talcum powder, 500-600 g of quartz powder, 2000-2500 g of fumed silica, 100-150 g of calcium oxide, 280-350 g of barium sulfate, 200-250 g of modified bentonite and 25-50 g of carbon black, mixing colors to grey, cooling to 20 ℃ and sealing and packaging under the protection of nitrogen.
1. The single-fluid anti-sagging non-expansion waterproof thermal insulation polyurethane material according to claim 1, wherein the polyurethane material is characterized in that: the stirring speed in the step 1 is regulated to be 70-90 revolutions per minute.
2. The single-fluid anti-sagging non-expansion waterproof thermal insulation polyurethane material according to claim 1, wherein the polyurethane material is characterized in that: in the step 2, toluene is clarified and cooled to below 60 ℃ and nitrogen is introduced for protection.
The single-fluid anti-sagging non-expansion waterproof thermal insulation polyurethane material according to claim 1, wherein the polyurethane material is characterized in that: and the quartz powder in the step 4 adopts 325-mesh quartz powder.
The invention has the beneficial effects that:
the waterproof performance of the polyurethane waterproof coating is superior to that of polyurethane waterproof coating on the market, the polyurethane waterproof coating can have heat preservation performance under the condition of no foaming, and the heat conductivity coefficient is low due to the fact that fumed silica is used in a large amount in the material, and the polyurethane waterproof coating can be waterproof and heat preservation at the same time; the invention has high breaking elongation and high breaking strength between the epoxy and the polyurea, and can be used as an anti-cracking buffer layer in concrete protection to well solve the problem of zero extension; the invention can reduce the construction cost and reduce the construction steps.
Detailed Description
The following examples are provided to further illustrate the invention.
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the detailed description is presented by way of example only and is not intended to limit the invention.
Example 1
A single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material comprises the following process steps:
s1, preparing hydroxyl-terminated polyether prepolymer: adding 210g of citric acid monohydrate, 580g of tripropylene glycol, 600g of dimethylbenzene and 15g of 98% concentrated sulfuric acid into a 2L flask, stirring, regulating the rotating speed to 70 revolutions per minute, heating to reflux, and separating water by a water separator; stopping heating when the water separated from the water separator is 72 ml; cooling to below 60 ℃ in air, adding 400ml of water, stirring for 5 minutes, pouring into a separating funnel, standing, discharging lower-layer liquid, adding water, and washing until the PH is greater than 6.5 to obtain an intermediate I;
s2, synthesizing polyether: adding 400g of dimethylbenzene into a 5L flask, stirring, adjusting the rotating speed to 90 r/min, heating to reflux, separating water by a water separator until the methylbenzene in the water separator is clarified, cooling to below 60 ℃, introducing nitrogen for protection, and adding 860g of 9 (ethoxy) trimethylolpropane to adjust the rotating speed to 90 r/min to obtain an intermediate II;
s3, synthesizing polyurethane resin: adding 0.8g of dibutyltin dilaurate and 15g of latent curing agent into an intermediate II, heating to 65 ℃, dropwise adding 330g of MDI (diphenylmethane diisocyanate), heating to reflux after the dropwise adding is completed, preserving heat for 2 hours, detecting the-NCO% in the mixture, and stopping the reaction when the-NCO% is 3.2%, thus obtaining resin I;
s4, manufacturing a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material: pouring the obtained resin I into a 10L high-speed stirrer to regulate the rotating speed to 150 revolutions per minute, preserving heat at 40 ℃, sequentially adding 80g of acetyl tributyl citrate, 18g of polyacrylamide, 100g of titanium white, 500g of talcum powder, 500g of 325-mesh quartz powder, 2000g of fumed silica, 100g of calcium oxide, 280g of barium sulfate, 200g of modified bentonite and 25g of carbon black, mixing colors until the temperature is reduced to 20 ℃ and sealing and packaging under the protection of nitrogen.
Example 2
A single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material comprises the following process steps:
s1, preparing hydroxyl-terminated polyether prepolymer: 250g of citric acid monohydrate, 640g of tripropylene glycol, 500g of dimethylbenzene and 10g of 98% concentrated sulfuric acid are added into a 2L flask for stirring, the rotating speed is regulated to 90 revolutions per minute, and then the mixture is heated to reflux, and the water separator is used for water diversion; stopping heating when the water separated from the water separator is 80 ml; cooling to below 60 ℃ in air, adding 400ml of water, stirring for 5 minutes, pouring into a separating funnel, standing, discharging lower-layer liquid, adding water, and washing until the PH is greater than 6.5 to obtain an intermediate I;
s2, synthesizing polyether: adding 450g of dimethylbenzene into a 5L flask, stirring, adjusting the rotating speed to 70 r/min, heating to reflux, separating water by a water separator until the methylbenzene in the water separator is clarified, cooling to below 60 ℃, introducing nitrogen for protection, and adding 900g of 9 (ethoxy) trimethylolpropane to adjust the rotating speed to 120 r/min to obtain an intermediate II;
s3, synthesizing polyurethane resin: adding 0.8g of dibutyltin dilaurate and 10g of latent curing agent into an intermediate II, heating to 85 ℃, dropwise adding 350g of MDI (diphenylmethane diisocyanate), heating to reflux after the dropwise adding is completed, preserving heat for 2 hours, detecting the-NCO% in the mixture, and stopping the reaction when the-NCO% is 3.8%, thus obtaining resin I;
s4, manufacturing a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material: pouring the obtained resin I into a 10L high-speed stirrer to regulate the rotation speed to 200 revolutions per minute, preserving heat at 50 ℃, sequentially adding 60g of acetyl tributyl citrate, 15g of polyacrylamide, 100g of titanium white, 550g of talcum powder, 600g of 325-mesh quartz powder, 2500g of fumed silica, 150g of calcium oxide, 350g of barium sulfate, 250g of modified bentonite and 50g of carbon black, mixing colors until the temperature is reduced to 20 ℃ and sealing and packaging under the protection of nitrogen.
Example 3
A single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material comprises the following process steps:
s1, preparing hydroxyl-terminated polyether prepolymer: adding 230g of citric acid monohydrate, 610g of tripropylene glycol, 550g of dimethylbenzene and 12g of 98% concentrated sulfuric acid into a 2L flask, stirring, adjusting the rotating speed to 80 revolutions per minute, heating to reflux, and separating water by a water separator; stopping heating when the water separated from the water separator is 77 ml; cooling to below 60 ℃ in air, adding 400ml of water, stirring for 5 minutes, pouring into a separating funnel, standing, discharging lower-layer liquid, adding water, and washing until the PH is greater than 6.5 to obtain an intermediate I;
s2, synthesizing polyether: adding 425g of dimethylbenzene into a 5L flask, stirring, adjusting the rotating speed to 80 r/min, heating to reflux, separating water by a water separator until the methylbenzene in the water separator is clarified, cooling to below 60 ℃, introducing nitrogen for protection, and adding 875g of 9 (ethoxy) trimethylolpropane to adjust the rotating speed to 110 r/min to obtain an intermediate II;
s3, synthesizing polyurethane resin: adding 0.8g of dibutyltin dilaurate and 12g of latent curing agent into an intermediate II, heating to 75 ℃, dropwise adding 330-350 g of MDI (diphenylmethane diisocyanate), heating to reflux after dropwise adding is completed, preserving heat for 2 hours, detecting-NCO% in the mixture, and stopping the reaction when the-NCO% is 3.5%, thus obtaining resin I;
s4, manufacturing a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material: pouring the obtained resin I into a 10L high-speed stirrer, regulating the rotating speed to 180 revolutions per minute, preserving heat at 45 ℃, sequentially adding 70g of acetyl tributyl citrate, 17g of polyacrylamide, 200g of titanium pigment, 520g of talcum powder, 530g of 325-mesh quartz powder, 2250g of fumed silica, 120g of calcium oxide, 310g of barium sulfate, 220g of modified bentonite and 40g of carbon black, mixing colors until the temperature is reduced to 20 ℃ and sealing and packaging under the protection of nitrogen.
In the above examples 1-3, xylene was used as the solvent, which was high in boiling point, and the reaction rate was accelerated; the consumption of the concentrated sulfuric acid relative to the benzenesulfonic acid catalyst is small and the subsequent cleaning is convenient; the nitrogen protection is used for removing water, so that the water is not involved in subsequent reactions; the-NCO% is controlled to be 3.2% -3.8%, and carbon dioxide can be generated as little as possible when the resin is subjected to moisture curing; 9 (ethoxy) trimethylolpropane can reduce the overall viscosity and has strong water absorption capacity; the latent curing agent adopts XY-3767 of Suzhou Xiangyuan New Material Co., ltd; the calcium oxide absorbs carbon dioxide generated by the reaction as much as possible under the condition of moisture, so that pores in the finished product are reduced, and the strength of the product is improved; the lower titanium dioxide is used for increasing the coverage rate.
In the invention, hydrophilic polyol is used as a main chain or a branched chain of resin to absorb water, and the hydrophilic polyol reacts with-NCO to harden after the resin contains water;
the invention relates to a single-component normal-temperature resin system which takes isocyanate resin as a base and is in a liquid state. The resin and water are hardened into a film by a chemical reaction of moisture curing, thereby producing a desired polymeric structure, and the hardened polymer exhibits excellent chemical resistance, mechanical properties and water-proof heat-insulating properties, and has excellent adhesion to many materials. This structure is not only advantageous in producing good processability. This system is proposed for: chemical building materials, water resistance and industrial aquaculture.
Basic characteristics of the present invention: the usable time (100 g/25 ℃) is 180 minutes; film drying time (15 g/3mm/25 ℃) for 420 minutes; shore A60 (15 g/3mm/25 ℃) cure hardness for 48 hours.
The method is influenced by a plurality of factors in the processing and using processes, and the applicability of the product is comprehensively tested before the product is used.
The storage of the invention should be sealed in the original packaging container, stored in clean and dry environment, placed in the dry place of 0-40 ℃ (the temperature cannot be lower than 0 ℃), and not stored in sunlight. The shelf life of the invention is 12 months from the date of production.
Comparison of the properties of examples 1-3 with those of the conventional materials on the market:
as can be seen from the table, the material prepared by the invention has more excellent characteristics than the traditional materials on the market.
The foregoing is merely illustrative of the present invention and not restrictive, and other modifications and equivalents thereof may occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (4)
1. The single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material is characterized by comprising the following process steps of:
s1, preparing hydroxyl-terminated polyether prepolymer: adding 210 g-250 g of citric acid monohydrate, 580 g-640 g of tripropylene glycol, 500 g-600 g of dimethylbenzene and 10 g-15 g of 98% concentrated sulfuric acid into a 2L flask, stirring, heating to reflux, and separating water by a water separator; stopping heating when the water separated from the water separator is 72 ml-80 ml; cooling to below 60 ℃ in air, adding 400ml of water, stirring for 5 minutes, pouring into a separating funnel, standing, discharging lower-layer liquid, adding water, and washing until the PH is greater than 6.5 to obtain an intermediate I;
s2, synthesizing polyether: adding 400-450 g of dimethylbenzene into a 5L flask, stirring, adjusting the rotating speed to 70-90 r/min, heating to reflux, separating water by a water separator until the methylbenzene in the water separator is clarified and cooled, introducing nitrogen for protection, and adding 860-900 g of 9 (ethoxy) trimethylolpropane to adjust the rotating speed to 90-120 r/min to obtain an intermediate II;
s3, synthesizing polyurethane resin: adding 0.8g of dibutyltin dilaurate and 10-15 g of latent curing agent into an intermediate II, heating to 65-85 ℃, dropwise adding 330-350 g of MDI (diphenylmethane diisocyanate), heating to reflux after the dropwise adding is completed, preserving heat for 2 hours, detecting the-NCO% in the mixture, and stopping the reaction when the-NCO% is 3.2-3.8%, thus obtaining resin I;
s4, manufacturing a single-liquid anti-sagging non-expansion waterproof heat-preservation polyurethane material: pouring the obtained resin I into a 10L high-speed stirrer to regulate the rotation speed to 150-200 r/min, preserving heat at 40-50 ℃, sequentially adding 60-80 g of acetyl tributyl citrate, 15-18 g of polyacrylamide, 100-250 g of titanium pigment, 500-550 g of talcum powder, 500-600 g of quartz powder, 2000-2500 g of fumed silica, 100-150 g of calcium oxide, 280-350 g of barium sulfate, 200-250 g of modified bentonite and 25-50 g of carbon black, mixing colors to grey, cooling to 20 ℃ and sealing and packaging under the protection of nitrogen.
2. The single-fluid anti-sagging non-expansion waterproof thermal insulation polyurethane material according to claim 1, wherein the polyurethane material is characterized in that: the stirring speed in the step 1 is regulated to be 70-90 revolutions per minute.
3. The single-fluid anti-sagging non-expansion waterproof thermal insulation polyurethane material according to claim 1, wherein the polyurethane material is characterized in that: in the step 2, toluene is clarified and cooled to below 60 ℃ and nitrogen is introduced for protection.
4. The single-fluid anti-sagging non-expansion waterproof thermal insulation polyurethane material according to claim 1, wherein the polyurethane material is characterized in that: and the quartz powder in the step 4 adopts 325-mesh quartz powder.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987940A (en) * | 2009-08-05 | 2011-03-23 | 任绍志 | Method for preparing high-performance single-component polyurethane waterproof coating |
| CN104530955A (en) * | 2014-12-23 | 2015-04-22 | 江苏凯伦建材股份有限公司 | Anti-sagging polyurethane waterproof coating |
| CN104877542A (en) * | 2015-06-16 | 2015-09-02 | 北京东方雨虹防水技术股份有限公司 | Mono-component PU (Polyurethane) root-resistant waterproof paint and preparation method thereof |
| CN110791165A (en) * | 2019-11-28 | 2020-02-14 | 河南东方雨虹建筑材料有限公司 | Single-component anti-sagging exposed modified polyurethane waterproof coating and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987940A (en) * | 2009-08-05 | 2011-03-23 | 任绍志 | Method for preparing high-performance single-component polyurethane waterproof coating |
| CN104530955A (en) * | 2014-12-23 | 2015-04-22 | 江苏凯伦建材股份有限公司 | Anti-sagging polyurethane waterproof coating |
| CN104877542A (en) * | 2015-06-16 | 2015-09-02 | 北京东方雨虹防水技术股份有限公司 | Mono-component PU (Polyurethane) root-resistant waterproof paint and preparation method thereof |
| CN110791165A (en) * | 2019-11-28 | 2020-02-14 | 河南东方雨虹建筑材料有限公司 | Single-component anti-sagging exposed modified polyurethane waterproof coating and preparation method thereof |
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