CN112430307A - Non-yellowing polyurethane sponge and preparation method thereof - Google Patents
Non-yellowing polyurethane sponge and preparation method thereof Download PDFInfo
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- CN112430307A CN112430307A CN202011328425.7A CN202011328425A CN112430307A CN 112430307 A CN112430307 A CN 112430307A CN 202011328425 A CN202011328425 A CN 202011328425A CN 112430307 A CN112430307 A CN 112430307A
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4816—Two or more polyethers of different physical or chemical nature mixtures of two or more polyetherpolyols having at least three hydroxy groups
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/143—Halogen containing compounds
- C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
- C08J9/145—Halogen containing compounds containing carbon, halogen and hydrogen only only chlorine as halogen atoms
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention provides a non-yellowing polyurethane sponge which is formed by a component A and a component B; the component A comprises: 70-90 parts by weight of a first polyether polyol; 10-30 parts by weight of a second polyether polyol; 1.5-4 parts by weight of water; 1-3 parts by weight of an amine catalyst; 1-3 parts by weight of a foam stabilizer; 0-10 parts by weight of a physical foaming agent; the component B comprises: 50-150 parts by weight of isocyanate; the number average molecular weight of the first polyether polyol is 5000-6000; the number average molecular weight of the second polyether polyol is 1000-3000. Compared with the prior art, the method takes the polyether polyol with low molecular weight as the pore-forming agent and combines the amine catalyst to ensure that the first polyether polyol can realize casting molding, avoids the yellowing phenomenon of the sponge in the processing and using processes, does not add whitening agent, antioxidant and the like, and does not pollute the fabric.
Description
Technical Field
The invention belongs to the technical field of polyurethane foaming, and particularly relates to a non-yellowing polyurethane sponge and a preparation method thereof.
Background
The polyurethane sponge is one kind of polyurethane foam plastic, belongs to soft polyurethane foam plastic, and is widely applied to the fields of clothing, packaging, automobiles, aviation, furniture and the like due to the advantages of low density, good elasticity, good air permeability, good water resistance, easily available raw materials and the like.
At present, most sponge manufacturers still use aromatic isocyanates such as Toluene Diisocyanate (TDI) and diphenylmethane diisocyanate (MDI) as raw materials, and since TDI and the isocyanate in MDI are directly connected based on benzene rings, yellowing and physical and mechanical properties are easily caused when the sponge manufacturers are exposed to the environment of illumination and nitrogen oxide for a long time.
In addition, the traditional bra sponge is formed by pressing sponge sheets on a cloth cup mold of a hot-press forming machine and heating the sponge sheets at high temperature to form the sponge into a cup shape. The sponge is easy to turn yellow in the processing and using processes, and the appearance is greatly influenced.
In order to maximally retard the yellowing of the sponge, a large amount of auxiliaries, such as antioxidants, ultraviolet absorbers, white pigments, etc., are added during the production process. Nevertheless, the sponge has a problem of yellowing during the hot press molding process.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a preparation method of alkyne-containing polyether modified silicone, which has the advantages of short reaction time, high conversion rate and less side reactions.
The invention provides a non-yellowing polyurethane sponge which is formed by a component A and a component B;
the component A comprises:
the component B comprises:
50-150 parts by weight of isocyanate;
the number average molecular weight of the first polyether polyol is 5000-6000;
the number average molecular weight of the second polyether polyol is 1000-3000.
Preferably, the first polyether polyol is prepared by taking ethylene oxide and propylene oxide as polymerization monomers; the mole number of the ethylene oxide is 8 to 15 percent of that of the polymerized monomer.
Preferably, the preparation of the second polyether polyol takes a second monomer as a polymerization monomer; the second monomer comprises ethylene oxide; the mole number of the ethylene oxide is 70-100% of that of the second monomer.
Preferably, the hydroxyl value of the first polyether polyol is 28-35; the hydroxyl value of the second polyether polyol is 28-35.
Preferably, the a component comprises:
preferably, the amine catalyst is selected from diamine catalysts;
the foam stabilizer is selected from organosilicon foam stabilizers;
the physical foaming agent is dichloromethane;
the isocyanate is selected from one or more of isophorone diisocyanate and modified products thereof.
Preferably, the amine catalyst is selected from diazabicyclo and/or its formic acid-modified delayed-action catalysts;
the foam stabilizer is selected from one or more of foam stabilizers with the trade names XH2836, XH2815 and XH2902 of Hangzhou Chongyao scientific and technological development Limited.
The invention also provides a preparation method of the non-yellowing polyurethane sponge, which comprises the following steps:
mixing the first polyether polyol, the second polyether polyol, water, the amine catalyst, the foam stabilizer and the physical foaming agent, stirring for the first time, then adding isocyanate, stirring for the second time, heating and drying to obtain the non-yellowing polyurethane sponge.
Preferably, after the second stirring, a polyurethane blend is obtained; and filling the polyurethane blend into a mold coated with a release agent, and heating and drying to obtain the non-yellowing polyurethane sponge.
Preferably, the rotating speed of the first stirring is 1000-1500 r/min; the first stirring time is 30-60 s; the rotation speed of the second stirring is 2500-3000 r/min; the time for the second stirring is 5-10 s; the temperature for heating and drying is 60-80 ℃; the heating and drying time is 5-10 min.
The invention provides a non-yellowing polyurethane sponge which is formed by a component A and a component B; the component A comprises: 70-90 parts by weight of a first polyether polyol; 10-30 parts by weight of a second polyether polyol; 1.5-4 parts by weight of water; 1-3 parts by weight of an amine catalyst; 1-3 parts by weight of a foam stabilizer; 0-10 parts by weight of a physical foaming agent; the component B comprises: 50-150 parts by weight of isocyanate; the number average molecular weight of the first polyether polyol is 5000-6000; the number average molecular weight of the second polyether polyol is 1000-3000. Compared with the prior art, the method takes the polyether polyol with low molecular weight as the pore-forming agent and combines the amine catalyst to ensure that the first polyether polyol can realize casting molding, avoids the yellowing phenomenon of the sponge in the processing and using processes, does not add whitening agent, antioxidant and the like, and does not pollute the fabric.
Experiments show that the whole density of the prepared non-yellowing polyurethane sponge is 55-60 Kg/m3The rebound resilience is 60-65%, the elongation at break is 120-150%, and the UV lamp does not turn yellow after being placed outside the UV lamp for 8 hours.
Drawings
FIG. 1 is a photograph of a polyurethane brassiere mold used in examples 1 to 3 of the present invention;
FIG. 2 is a photograph of a mold for a polyurethane brassiere used in examples 1 to 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a non-yellowing polyurethane sponge which is formed by a component A and a component B;
the component A comprises:
the component B comprises:
50-150 parts by weight of isocyanate;
the number average molecular weight of the first polyether polyol is 5000-6000;
the number average molecular weight of the second polyether polyol is 1000-3000.
The invention takes polyether polyols with different molecular weights as the polyol raw material of the polyurethane sponge.
The content of the first polyether polyol is preferably 75-85 parts by weight, and more preferably 80 parts by weight; the first polyether polyol is prepared by taking ethylene oxide and propylene oxide as polymerization monomers; the mole number of the ethylene oxide is preferably 8 to 15 percent of that of the polymerized monomer; the first polyether polyol is preferably prepared by taking glycerol as an initiator; the hydroxyl value of the first polyether polyol is preferably 28-35; the unsaturation of the first polyether polyol is preferably less than 0.1%.
In the polyurethane sponge provided by the invention, the second polyether polyol is used as a cell opening agent at the same time, so that the surface tension of the foam can be reduced, the cell breakage can be promoted, the cell opening rate of the polyurethane foam can be improved, and the softness caused by closed cells can be improved. The content of the second polyether polyol is preferably 15-25 parts by weight, and more preferably 20 parts by weight; the preparation of the second polyether polyol preferably takes a second monomer as a polymerization monomer; the second monomer comprises ethylene oxide; the mole number of the epoxy resin is 70-100% of that of the second monomer; namely, the invention uses polyether polyol which takes ethylene oxide as a main body and is subjected to ring-opening polymerization as a cell opening agent; the second polyether polyol is preferably prepared by taking glycerol as an initiator; the number average molecular weight of the second polyether polyol is preferably 1500-2500, and more preferably 2000; the hydroxyl value of the second polyether polyol is preferably 28-35; the unsaturation of the second polyether polyol is preferably less than 0.1%.
According to the present invention, the water is preferably contained in an amount of 2 to 3.5 parts by weight, more preferably 2 to 3 parts by weight, and still more preferably 2 to 2.4 parts by weight.
The content of the amine catalyst is preferably 1 to 2.5 parts by weight, more preferably 1 to 2 parts by weight, and still more preferably 1.3 to 1.6 parts by weight; the amine catalyst is preferably a diamine catalyst, more preferably a Diazabicyclo (DBU) and/or its formic acid-modified delayed-action catalyst; when a mixture of a Diazabicyclo (DBU) and a formic acid-modified delayed-action catalyst thereof is used as the amine-based catalyst, the mass ratio of the Diazabicyclo (DBU) to the formic acid-modified delayed-action catalyst thereof is preferably (10 to 15): 3, more preferably (12-14): 3, more preferably 13: 3.
the content of the foam stabilizer is preferably 1-2.5 parts by weight, more preferably 1-2 parts by weight, and still more preferably 1.2-1.6 parts by weight; the foam stabilizer is preferably an organic silicon foam stabilizer, more preferably one or more foam stabilizers with the trade names XH2836, XH2815 and XH2902 of Chongzhou Chongyao scientific and technological development Limited, and further preferably XH2836 and XH 2815; the mass ratio of XH2836 to XH2815 is preferably (2-3): 1.
the present invention may also include a physical blowing agent; the physical blowing agent is preferably methylene chloride.
According to the invention, the content of the polyurethane is preferably 60 to 120 parts by weight, more preferably 70 to 100 parts by weight, still more preferably 70 to 90 parts by weight, and most preferably 74 to 88 parts by weight; the polyurethane has a structure of OCN-R-NCO, wherein R represents an isocyanate nuclear group; to further improve the yellowing resistance of the foamed article; in the present invention, one or more of isophorone diisocyanate and its modifications are preferably used; the structural formula of the isophorone diisocyanate is as follows:
the invention takes the polyether glycol with low molecular weight as the pore-forming agent and combines the amine catalyst to ensure that the first polyether glycol can realize casting molding, avoids the yellowing phenomenon of the sponge in the processing and using processes, does not add whitening agent, antioxidant and the like, and does not pollute the fabric.
The invention also provides a preparation method of the non-yellowing polyurethane sponge, which comprises the following steps: mixing the first polyether polyol, the second polyether polyol, water, the amine catalyst, the foam stabilizer and the physical foaming agent, stirring for the first time, then adding isocyanate, stirring for the second time, heating and drying to obtain the non-yellowing polyurethane sponge.
The invention has no special limitation on the sources of all the raw materials, and the raw materials are available on the market; the first polyether polyol, the second polyether polyol, water, the amine catalyst, the foam stabilizer, the physical foaming agent and the isocyanate are the same as described above, and are not described again.
Mixing the first polyether polyol, the second polyether polyol, water, an amine catalyst, a foam stabilizer and a physical foaming agent, and stirring for the first time to obtain a component A; the rotating speed of the first stirring is preferably 1000-1500 r/min; the time for the first stirring is preferably 30 to 60 seconds, more preferably 40 to 50 seconds, and still more preferably 45 seconds.
Then adding isocyanate and stirring for the second time to obtain a polyurethane blend; the rotation speed of the second stirring is preferably 2500-3000 r/min; the time for the second stirring is preferably 5 to 10s, more preferably 6 to 8s, and still more preferably 7 s.
In the present invention, it is preferable that the polyurethane blend is filled into a mold and then dried by heating to obtain a non-yellowing polyurethane sponge; the heating and drying temperature is preferably 60-80 ℃; the heating and drying time is preferably 5-10 min; the reaction process comprises the following steps:
①-NCO+H2O→-NH2+CO2↑
②-NCO+-OH→-HNCOO-
in the present invention, it is more preferable to fill into a mold coated with a release agent; the release agent can be an organic release agent or an oily release agent, and the oily release agents LK 706 and/or LK 888 provided by Evonik are preferably used in the invention; in order to further improve the air permeability of the non-yellowing polyurethane sponge; the inner surface of the mould is preferably provided with steel nails; the length of the steel nail is preferably 1-5 mm.
The non-yellowing polyurethane sponge provided by the invention can be obtained by a one-step casting molding method, high-temperature hot press molding is not needed, and the product does not contain high-temperature derived toxic gas; and a whitening agent, an antioxidant and the like are not added, so that the fabric is not polluted.
In order to further illustrate the present invention, the following will describe a non-yellowing polyurethane sponge and a method for preparing the same in detail with reference to the examples.
The reagents used in the following examples are all commercially available;
in the embodiment, the first polyether polyol is Tianjin petrochemical 330N, glycerol is used as an initiator, ethylene oxide and propylene oxide are used as polymerization monomers, the content of the ethylene oxide is 8-15%, the molecular weight of the first polyether polyol is 5000-6000, the hydroxyl value is 28-35, and the unsaturation degree is lower than 0.1%;
the second polyether polyol is Shandong Lanxing polyether, glycerin is used as an initiator, ethylene oxide and propylene oxide are used as polymerization monomers, the content of the ethylene oxide is 70% -100%, the molecular weight of the second polyether polyol is 5000-6000, the hydroxyl value is 28-35, and the degree of unsaturation is lower than 0.1%;
the foam stabilizer is an interworking system (mass ratio of 2:1-3:1) of Hangzhou Chongyao organosilicon surfactant XH2836 and XH2815 with special structural design.
Example 1
The formula of the polyurethane sponge comprises:
mixing the first polyether polyol, the second polyether polyol, water, an amine catalyst and a foam stabilizer for 1000r/min, stirring for 45s, adding the isocyanate for 2500r/min, and stirring at a high speed for 7s to obtain the polyurethane blend.
Heating a sponge bra mold (see figures 1 and 2, which are photographs of the sponge bra mold) to 60 ℃, coating an oily release agent LK 706 provided by Evonik inside the sponge bra mold, putting the sponge bra mold into a heating drying box, keeping the temperature to 60 ℃, pouring the polyurethane blend prepared by the formula into the sponge bra mold, covering the mold, putting the sponge bra mold into the heating drying box, preserving the heat for 8 minutes, and demolding to obtain the bra cup with fine and smooth foam pores and a smooth surface.
Example 2
The formula of the polyurethane sponge comprises:
according to the production process flow of the embodiment 1, the bra cup with fine foam holes and smooth surface is obtained.
Example 3
The formula of the polyurethane sponge comprises:
according to the production process flow of the embodiment 1, the bra cup with fine foam holes and smooth surface is obtained.
Compared with yellowing resistance of products, the polyurethane bra sponge prepared in the embodiments 1 to 3 and common bra cotton (the existing bra cup is a sponge prepared from polyether polyol and TDI/MDI, a sponge sheet and cloth are compounded by glue, then a hot-press forming machine is used for pressing on a cloth cup mold, and the sponge is heated at high temperature to enable the sponge to flow into a cup shape) are placed under an ultraviolet lamp together, the common bra cotton becomes slightly yellow after 2 hours, and the foam process is burnt yellow after 8 hours, but the color of the product obtained according to the invention is basically not changed.
The performance of the polyurethane bra sponges obtained in examples 1-3 was tested and the results are shown in table 1.
TABLE 1 detection results of the properties of polyurethane bra sponge
| Bulk density | Rebound resilience | Elongation at break | |
| Example 1 | 57.4 | 64 | 125.5 |
| Example 2 | 56.2 | 61 | 133.2 |
| Example 3 | 56.8 | 62 | 130.5 |
Claims (10)
1. The non-yellowing polyurethane sponge is characterized by being formed by a component A and a component B;
the component A comprises:
the component B comprises:
50-150 parts by weight of isocyanate;
the number average molecular weight of the first polyether polyol is 5000-6000;
the number average molecular weight of the second polyether polyol is 1000-3000.
2. The non-yellowing polyurethane sponge according to claim 1, wherein the first polyether polyol is prepared by using ethylene oxide and propylene oxide as polymerization monomers; the mole number of the ethylene oxide is 8 to 15 percent of that of the polymerized monomer.
3. The non-yellowing polyurethane sponge according to claim 1, wherein the second polyether polyol is prepared by using a second monomer as a polymerization monomer; the second monomer comprises ethylene oxide; the mole number of the ethylene oxide is 70-100% of that of the second monomer.
4. The non-yellowing polyurethane sponge according to claim 1, wherein the first polyether polyol has a hydroxyl number of 28 to 35; the hydroxyl value of the second polyether polyol is 28-35.
5. The non-yellowing polyurethane sponge according to claim 1, wherein the A component comprises:
6. the non-yellowing polyurethane sponge according to claim 1, wherein the amine catalyst is selected from the group consisting of diamine catalysts;
the foam stabilizer is selected from organosilicon foam stabilizers;
the physical foaming agent is dichloromethane;
the isocyanate is selected from one or more of isophorone diisocyanate and modified products thereof.
7. The non-yellowing polyurethane sponge according to claim 1, wherein the amine catalyst is selected from diazabicyclo and/or its formic acid-modified delayed catalyst;
the foam stabilizer is selected from one or more of foam stabilizers with the trade names XH2836, XH2815 and XH2902 of Hangzhou Chongyao scientific and technological development Limited.
8. A method of preparing the non-yellowing polyurethane sponge of claim 1, comprising:
mixing the first polyether polyol, the second polyether polyol, water, the amine catalyst, the foam stabilizer and the physical foaming agent, stirring for the first time, then adding isocyanate, stirring for the second time, heating and drying to obtain the non-yellowing polyurethane sponge.
9. The method of claim 8, wherein after the second stirring, a polyurethane blend is obtained; and filling the polyurethane blend into a mold coated with a release agent, and heating and drying to obtain the unchanged polyurethane sponge.
10. The preparation method according to claim 8, wherein the rotation speed of the first stirring is 1000 to 1500 r/min; the first stirring time is 30-60 s; the rotation speed of the second stirring is 2500-3000 r/min; the time for the second stirring is 5-10 s; the temperature for heating and drying is 60-80 ℃; the heating and drying time is 5-10 min.
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| CN109535382A (en) * | 2018-10-18 | 2019-03-29 | 青岛中和聚氨酯材料有限公司 | A kind of non yellowing polyurethane sponge and preparation method thereof |
| CN110305289A (en) * | 2019-07-29 | 2019-10-08 | 福建大方睡眠科技股份有限公司 | A kind of non yellowing polyurethane memory cotton and preparation method thereof |
| CN111040113A (en) * | 2019-12-27 | 2020-04-21 | 江苏世丰新材料有限公司 | Hydrophilic sponge material and preparation method thereof |
| CN111393833A (en) * | 2020-04-02 | 2020-07-10 | 张家港长泰汽车饰件材料有限公司 | High-opening-rate hydrolysis-resistant polyurethane foam and preparation method and application thereof |
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