CN111777852B - Preparation method of polyurethane foam gap filler - Google Patents

Preparation method of polyurethane foam gap filler Download PDF

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Publication number
CN111777852B
CN111777852B CN202010510228.0A CN202010510228A CN111777852B CN 111777852 B CN111777852 B CN 111777852B CN 202010510228 A CN202010510228 A CN 202010510228A CN 111777852 B CN111777852 B CN 111777852B
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preparation
curing agent
polyurethane foam
gap filler
aerosol
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CN111777852A (en
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陈士强
朱强
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Suzhou Geno New Material Technology Co ltd
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Suzhou Geno New Material Technology Co ltd
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Abstract

The invention relates to a preparation method of a polyurethane foam gap filler, which mainly comprises the preparation of a curing agent, the preparation of combined polyether and the preparation of the polyurethane foam gap filler, wherein the preparation of the curing agent comprises the following steps: mixing 2, 2-dimethylolpropionic acid and 1,1, 1-trimethylolpropane, stirring, heating to 140-150 ℃, reacting for 15-30 min, pressurizing to 10MPa, adding propenyl-1, 3-sultone and methylbenzenesulfonic acid, reacting for 3h, and decompressing to atmospheric pressure; adding the combined polyether and the curing agent into an aerosol can, filling dimethyl ether, shaking and standing at room temperature. By adding the self-made curing agent, the curing speed is improved after filling.

Description

Preparation method of polyurethane foam gap filler
Technical Field
The invention relates to the technical field of sealing materials, in particular to a preparation method of a polyurethane foam gap filler.
Background
The ammonia-vinegar foam joint mixture is commonly called foaming agent, foaming glue and PU joint mixture, and is a product of cross combination of an aerosol technology and a polyurethane foam technology. When the material is sprayed from the aerosol canister, the foamed polyurethane material expands rapidly and undergoes a curing reaction with air or moisture in the substrate in contact therewith to form a foam. The cured polyurethane foam gap filler foam has multiple effects of gap filling, bonding, sealing, sunlight heating, sound absorption and the like, is an environment-friendly and energy-saving building material convenient to use, can be suitable for sealing, leaking stoppage, filling gaps, fixing bonding, preserving heat and insulating sound, is particularly suitable for sealing, leaking stoppage and waterproofing between plastic steel or aluminum alloy doors and windows and walls, and is more and more widely used.
The existing polyurethane gap filler has the defects of low curing speed after gap filling, poor mechanical strength, influence on construction quality, frequent need of rework and unnecessary trouble.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a polyurethane foam gap filler with high curing speed and high mechanical strength.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the polyurethane foam gap filler comprises the preparation of a curing agent, the preparation of combined polyether and the preparation of the polyurethane foam gap filler, wherein the preparation of the curing agent comprises the following steps: mixing 2, 2-dimethylolpropionic acid and 1,1, 1-trimethylolpropane, stirring and heating to 140-150 ℃, reacting for 15-30 min, increasing the pressure to 10MPa, then adding propenyl-1, 3-sultone and methylbenzenesulfonic acid, reacting for 3h, and reducing the pressure to atmospheric pressure;
adding the combined polyether and the curing agent into an aerosol can, filling dimethyl ether, shaking and standing at room temperature.
The raw material ratio of the curing agent is as follows:
80-90 g of 2, 2-dimethylolpropionic acid
60-70 g of 1,1, 1-trimethylolpropane
2-3 g of propenyl-1, 3-sultone
3.0-5.0 mL of methylbenzenesulfonic acid
The preparation process of the combined polyether comprises the following steps: 100-120 g of polyether polyol with the functionality of 2, 70-80 g of polyester polyol with the functionality of 2, 80-100 g of chlorinated paraffin, 10-15 g of catalyst, 1-3 g of pentamethyldiethylenetriamine and 20-30 g of hard particles are shaken and mixed for 0.5h, and the mixture is mixed uniformly.
The hard particles comprise silicon dioxide, magnesium phosphate, aluminum hydroxide and borax with the particle size of 10-15 microns.
The preparation process of the polyurethane foam gap filler comprises the following steps: adding 300-350 g of combined polyether, 10-20 g of curing agent, 240-250 g of polymethyl isoamino acid ester and 8-10 g of organic silicone into a 1000mL aerosol can, filling 50-60 g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain the finished product.
Compared with the prior art, the invention has the beneficial effects that: by adding the self-made curing agent, the curing speed is improved after filling; by adding hard particles, the mechanical strength is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention relates to a preparation method of a polyurethane foam gap filler, which mainly comprises the following steps of preparation of a curing agent, preparation of combined polyether and preparation of the polyurethane foam gap filler:
synthesis of curing agent
Under the protection of nitrogen, adding 80-90 g of 2, 2-dimethylolpropionic acid and 60-70 g of 1,1, 1-trimethylolpropane into a 500mL reaction vessel, mechanically stirring and heating to 140-150 ℃, reacting for 15-30 min, raising the pressure to 10MPa, then adding 2-3 g of propenyl-1, 3-sultone into the reaction vessel, adding 3.0-5.0 mL of methylbenzenesulfonic acid as a catalyst, reacting for 3h, and reducing the pressure to atmospheric pressure to obtain the curing agent.
Preparation of conjugate polyether
100-120 g of polyether polyol with the functionality of 2, 70-80 g of polyester polyol with the functionality of 2, 80-100 g of chlorinated paraffin, 10-15 g of catalyst, 1-3 g of pentamethyldiethylenetriamine and 20-30 g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Wherein the hard particles comprise silicon dioxide, magnesium phosphate, aluminum hydroxide and borax with the particle size of 10-15 microns.
Preparation of polyurethane foam gap filler
Adding 300-350 g of combined polyether, 10-20 g of curing agent, 240-250 g of polymethyl isoamino acid ester and 8-10 g of organic silicone into a 1000mL aerosol can, filling 50-60 g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Example 1
Synthesis of curing agent
Under the protection of nitrogen, 90g of 2, 2-dimethylolpropionic acid and 60g of 1,1, 1-trimethylolpropane are added into a reaction vessel, the mixture is mechanically stirred and heated to 150 ℃, the reaction is carried out for 15min, the pressure is increased to 10MPa, then 3g of propenyl-1, 3-sultone is added into the reaction vessel, 4.0mL of methyl benzenesulfonic acid is added as a catalyst, the reaction is carried out for 4h, and the pressure is reduced to atmospheric pressure, so that the curing agent is obtained.
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 100g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 25g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 10g of curing agent, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Example 2
Synthesis of curing agent
Under the protection of nitrogen, 85g of 2, 2-dimethylolpropionic acid and 70g of 1,1, 1-trimethylolpropane are added into a reaction vessel, the mixture is mechanically stirred and heated to 145 ℃, the reaction is carried out for 20min, the pressure is increased to 10MPa, then 2g of propenyl-1, 3-sultone is added into the reaction vessel, 5.0mL of methyl benzenesulfonic acid is added as a catalyst, the reaction is carried out for 3h, and the pressure is reduced to atmospheric pressure, thus obtaining the curing agent.
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 80g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 20g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 15g of curing agent, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Example 3
Synthesis of curing agent
Under the protection of nitrogen, 80g of 2, 2-dimethylolpropionic acid and 65g of 1,1, 1-trimethylolpropane are added into a reaction vessel, the mixture is mechanically stirred and heated to 140 ℃, the reaction is carried out for 30min, the pressure is increased to 10MPa, then 3g of propenyl-1, 3-sultone is added into the reaction vessel, 5.0mL of methyl benzenesulfonic acid is added as a catalyst, the reaction is carried out for 3h, and the pressure is reduced to atmospheric pressure, so that the curing agent is obtained.
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 90g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 25g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 20g of curing agent, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Example 4
Synthesis of curing agent
Under the protection of nitrogen, 90g of 2, 2-dimethylolpropionic acid and 60g of 1,1, 1-trimethylolpropane are added into a reaction vessel, the mixture is mechanically stirred and heated to 150 ℃, the reaction is carried out for 15min, the pressure is increased to 10MPa, then 3g of propenyl-1, 3-sultone is added into the reaction vessel, 4.0mL of methyl benzenesulfonic acid is added as a catalyst, the reaction is carried out for 4h, and the pressure is reduced to atmospheric pressure, so that the curing agent is obtained.
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 90g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 30g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 15g of curing agent, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Example 5
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 90g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 30g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain the finished product.
Example 6
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 90g of chlorinated paraffin, 13g of catalyst and 2g of pentamethyldiethylenetriamine are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain the finished product.
Example 7
Synthesis of curing agent
Under the protection of nitrogen, 80g of 2, 2-dimethylolpropionic acid and 65g of 1,1, 1-trimethylolpropane are added into a reaction vessel, the mixture is mechanically stirred and heated to 140 ℃, the reaction is carried out for 30min, then 3g of propenyl-1, 3-sultone is added into the reaction vessel, 5.0mL of methyl benzenesulfonic acid is added as a catalyst, and the reaction is carried out for 3h under normal pressure, so as to obtain the curing agent.
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 90g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 25g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 20g of curing agent, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Example 8
Synthesis of curing agent
Under the protection of nitrogen, 80g of 2, 2-dimethylolpropionic acid and 65g of 1,1, 1-trimethylolpropane are added into a reaction vessel, the mixture reacts for 30min at normal temperature, the pressure is increased to 10MPa, then 3g of propenyl-1, 3-sulfoacid lactone is added into the reaction vessel, 5.0mL of methyl benzenesulfonic acid is added as a catalyst, the reaction is carried out for 3h, and the pressure is reduced to atmospheric pressure, so that the curing agent is obtained.
Preparation of conjugate polyether
110g of polyether polyol with the functionality of 2, 75g of polyester polyol with the functionality of 2, 90g of chlorinated paraffin, 13g of catalyst, 2g of pentamethyldiethylenetriamine and 25g of hard particles are shaken and mixed for 0.5h, and the combined polyether is prepared after even mixing.
Preparation of polyurethane foam gap filler
And adding 325g of combined polyether, 20g of curing agent, 245g of polymethyl isoamino acid ester and 9g of organic silicone into a 1000mL aerosol can, filling 55g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product.
Data result comparison statistical table for embodiments 1-8 of the invention
TABLE 1
Examples Curing time (min) Tensile Strength (Kpa)
Example 1 16 0.46
Example 2 20 0.58
Example 3 13 0.55
Example 4 18 0.43
Example 5 40 0.41
Example 6 35 0.33
Example 7 30 0.38
Example 8 50 0.43
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (1)

1. The preparation method of the polyurethane foam gap filler is characterized by comprising the following steps:
the preparation process of the polyurethane foam gap filler comprises the following steps: adding 300-350 g of combined polyether, 10-20 g of curing agent, 240-250 g of polymethyl isoamino acid ester and 8-10 g of organic silicone into a 1000mL aerosol can, filling 50-60 g of dimethyl ether on an aerosol filling machine, shaking for 3min, and standing at room temperature for 24h to obtain a finished product;
the raw material ratio of the curing agent is as follows:
80-90 g of 2, 2-dimethylolpropionic acid
60-70 g of 1,1, 1-trimethylolpropane
2-3 g of propenyl-1, 3-sultone
3.0-5.0 mL of methylbenzenesulfonic acid;
the preparation process of the curing agent comprises the following steps: mixing 2, 2-dimethylolpropionic acid and 1,1, 1-trimethylolpropane, stirring, heating to 140-150 ℃, reacting for 15-30 min, pressurizing to 10MPa, adding propenyl-1, 3-sultone and methylbenzenesulfonic acid, reacting for 3h, and decompressing to atmospheric pressure;
the preparation process of the combined polyether comprises the following steps: 100-120 g of polyether polyol with the functionality of 2, 70-80 g of polyester polyol with the functionality of 2, 80-100 g of chlorinated paraffin, 10-15 g of catalyst, 1-3 g of pentamethyldiethylenetriamine and 20-30 g of hard particles are shaken and mixed for 0.5h, and the mixture is mixed uniformly;
the hard particles comprise silicon dioxide, magnesium phosphate, aluminum hydroxide and borax, and the particle size of the silicon dioxide is 10-15 micrometers.
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Denomination of invention: Preparation method of polyurethane foam sealant

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