CN111961184A - Low-density ultraviolet radiation-resistant polyurethane sponge and preparation method thereof - Google Patents
Low-density ultraviolet radiation-resistant polyurethane sponge and preparation method thereof Download PDFInfo
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- CN111961184A CN111961184A CN201910416311.9A CN201910416311A CN111961184A CN 111961184 A CN111961184 A CN 111961184A CN 201910416311 A CN201910416311 A CN 201910416311A CN 111961184 A CN111961184 A CN 111961184A
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- 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
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
- C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
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- 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
- C08G18/08—Processes
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- 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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- 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
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
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- 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
- C08J9/0066—Use of inorganic compounding ingredients
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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
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- 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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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2101/00—Manufacture of cellular products
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/08—Polyurethanes from polyethers
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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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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Abstract
The invention provides ultraviolet radiation resistant polyurethane sponge and a preparation method thereof, wherein the ultraviolet radiation resistant polyurethane sponge comprises the following components in parts by weight: 100 parts of polyether polyol, 2-15 parts of tetrabutyl titanate, 0.1-10 parts of tributyl citrate, 4-9 parts of water, 0.05-0.2 part of amine catalyst, 0.1-0.4 part of organic tin catalyst, 1.0-3.0 parts of foam stabilizer, 8-20 parts of dichloromethane and 50-65 parts of TDI. The low-density polyurethane sponge prepared by the invention has better pore distribution, and the sponge height is not influenced; no release agent is needed, and the cured product can completely fall off from the die and has better ultraviolet resistance.
Description
Technical Field
The invention belongs to the technical field of polyurethane sponge production, and relates to a low-density ultraviolet irradiation resistant polyurethane sponge and a preparation method thereof.
Background
Polyurethane sponge products have become popular in people's lives, and among them, there are household articles such as chairs, sofas, mattresses, etc. made of sponge. In the polyurethane sponge industry, TDI (toluene diisocyanate) is a main raw material for producing polyurethane sponge, and TDI (toluene diisocyanate) has a benzene ring, so that free radical transition is very easy to occur under the condition of ultraviolet irradiation, the structure of TDI is damaged, the color is yellow, the appearance is influenced, and even the mechanical property is reduced.
The existing sponge prepared from isocyanate and polyether polyol is generally resistant to ultraviolet rays by adding organic stabilizers, such as the use of the hindered phenol as an antioxidant stabilizer and the hindered amine as a light stabilizer mentioned in CN103923292A, and these stabilizers have certain physiological toxicity and volatility and can cause harm to human health, on the other hand, these compounds can also cause damage to the environment, and in some application fields or countries, these stabilizers are restricted by relevant laws and regulations.
In the low-density sponge industry, the phenomena of uneven distribution of sponge pores, large and obvious part of pores and the like often occur in the field of box foams in common physical foaming agents such as dichloromethane (MC) and the like, so that the product quality is influenced. Sponges generally exhibit strong sticking and tend to result in incomplete foam upon demolding.
In the prior art, the uniformity of the pores in the sponge foam is generally adjusted by adding a foam stabilizer silicone oil, and as mentioned in CN106700030A, silicone oil is used as a foam stabilizer and a cell opener. However, in many cases, the silicone oil content is increased, which often results in the reduction of foam height and affects the sponge output rate. The low-density sponge generally has a mold sticking phenomenon, and even if a mold is treated by using a mold release agent in advance, the process is additionally increased, the cost is increased, and the effect is not necessarily obvious.
In view of the shortcomings of the prior art, there is a need to develop a new polyurethane sponge.
Disclosure of Invention
One of the objectives of the present invention is to provide a low-density uv-resistant polyurethane sponge in response to the above problems of the prior art. The low-density polyurethane sponge prepared by the invention has better pore distribution, and the sponge height is not influenced; a release agent is not needed in the preparation process, and the cured product can completely fall off from the mold; has better ultraviolet irradiation resistance, and the ultraviolet resistant additive is environment-friendly.
Another object of the present invention is to provide a method for preparing the polyurethane sponge.
The purpose of the invention can be realized by the following technical scheme:
a low-density ultraviolet radiation resistant polyurethane sponge has a density of 10-18kg/m3The formula comprises the following components in parts by weight:
the polyether polyol is low-odor polyether polyol which is prepared by ring-opening polymerization of ethylene oxide and propylene oxide by taking glycerol and/or trimethylolpropane as an initiator. The unsaturation degree of the polyether polyol is less than 0.05mol/kg, the number average molecular weight is 3000-6000, and the molecular weight distribution is less than 1.05; wherein the proportion of the ethylene oxide content in the mass of the polyether polyol is 5-30 wt% based on the total mass of the polyether polyol.
The polyether polyol of the present invention includes, but is not limited to, one or more of F3135 from Wanhua chemical group, Inc., GEP-330N from high petrochemical, FA-703 from Coria, EP-330NY from Shandong Lanxingdong chemical company, Inc., 3010 from DOW, F3156 from Wanhua chemical group, Inc., DEP-561D from Lanxindong Datoward Inc., PPG-5623 from Shell, GEP-560s from high petrochemical, etc., preferably F3156 and/or F3135 from Wanhua chemical group.
The amine catalyst can be triethylene diamine and/or bis (dimethylaminoethyl) ether.
The organotin catalyst may be stannous octoate and/or dibutyltin dilaurate.
The foam stabilizer is silicone oil, preferably one or more of creative silicone oil B8180, B8123, B8110 and B8170.
In the formula of the polyurethane sponge, tetrabutyl titanate can quickly react with part of water in a foaming system to hydrolyze to generate titanium dioxide hydrate, and the titanium dioxide hydrate has no volatility and tolerance, so that the sponge has ultraviolet resistance and does not cause harm to the environment.
The invention also discloses a preparation method of the ultraviolet radiation resistant polyurethane sponge, which comprises the following steps of:
(1) premixing: premixing 40-60% of dehydrated polyether polyol with the whole amount of tetrabutyl titanate and the whole amount of tributyl citrate, and uniformly stirring to obtain a premix;
(2) stirring the milk white: conveying the premix and the rest components to a mixing device for mixing, quickly pouring the mixture into a mold after uniformly stirring, and observing the thick liquid which is changed from semitransparent to full turbid and whitish;
(3) and (3) gel: the rising foam was observed to stop growing and a large number of bubbles were expelled from the skin, after a period of time the foam height stopped changing.
(4) Curing: and (3) placing the gelled sponge in a shading and ventilating environment for standing for a certain time to obtain the required product.
In the preparation method of the polyurethane sponge, in the step (1), the water content of the dehydrated polyether polyol is less than 200ppm, preferably less than 160 ppm. The dehydration of the polyether polyol is a process conventional in the art, such as distillation under reduced pressure. In the step (1), the stirring time is 20-40 s.
In the step (2), the stirring time is 5-10 s.
In the step (3), the time from the stop of the increase of the foam body to the stop of the change of the foam height is called gel time, and the gel time is 100-700 s.
In the step (4), the curing temperature is 25-40 ℃, and the curing time is 1-9 days.
According to the polyurethane sponge, the tributyl citrate can be partially dispersed on the bonding surface of the foam and the mold, so that the bonding phenomenon of the foam and the mold is effectively reduced, the product has good self-demolding capacity, the preparation process is simplified, and the production cost is reduced; the tetrabutyl titanate hydrolysate and the tributyl citrate form tiny particles which are uniformly distributed in the foam under the action of high-speed stirring, so that the silicone oil can be assisted to ensure that foam pores are more uniform and fine, the dosage of the silicone oil is reduced, and the foam height is not influenced.
Compared with the prior art, the ultraviolet radiation resistant polyurethane sponge has the following advantages:
(1) in the invention, the tributyl citrate dispersed on the bonding surface of the foam and the mold effectively reduces the bonding phenomenon of the foam and the mold and shows good self-demolding capability;
(2) according to the invention, the tetrabutyl titanate hydrolysate and the tributyl citrate are stirred at a high speed to form tiny particles which are uniformly distributed in the foam, so that silicone oil can be assisted to enable foam pores to be more uniform and fine without affecting the foam height;
(3) in the invention, tetrabutyl titanate and part of water in a foaming system react rapidly to hydrolyze to generate titanium dioxide hydrate, which has no volatility, so that the foam has ultraviolet resistance and no harm to the environment;
(4) the preparation method is simple, has low requirements on equipment and has low total cost.
Detailed Description
The invention is further illustrated by the following examples, but is not limited thereto.
Examples 1 to 4 and comparative examples 1 to 2
The ultraviolet radiation resistant polyurethane sponge comprises the following components in parts by weight:
TABLE 1 examples and comparative examples are as follows
| Comparative example 1 | Comparative example 2 | Example 1 | Example 2 | Example 3 | Example 4 | |
| Polyether polyol F3156 | 100 | 100 | 100 | 100 | 100 | 100 |
| Tetrabutyl titanate | 6 | 6 | 10 | 2.5 | 14 | |
| Citric acid tributyl ester | 0.5 | 8 | 5 | 1.2 | ||
| Water (W) | 5 | 5 | 5 | 8 | 9 | 7 |
| Triethylene diamine | 0.13 | 0.1 | 0.13 | 0.1 | 0.05 | 0.07 |
| Stannous octoate | 0.1 | 0.1 | 0.1 | 0.4 | 0.3 | 0.2 |
| Silicone oil B8123 | 2 | 2 | 2 | 1.5 | 2 | 2.5 |
| Methylene dichloride | 16 | 16 | 16 | 10 | 15 | 9 |
| TDI | 52 | 52 | 52 | 60 | 65 | 55 |
The preparation method of the ultraviolet radiation resistant polyurethane sponge comprises the following steps:
(1) premixing: premixing 50 parts of dehydrated polyether polyol F3156 with the water content of 180ppm with tetrabutyl titanate and tributyl citrate, stirring for 35 seconds, and uniformly mixing to obtain a premix as a single component;
(2) stirring the milk white: conveying the premix and the rest components to a mixing device according to the metering of the formula for mixing, stirring for 8s by a machine head, uniformly mixing, quickly pouring the mixture into a mold, and observing the thick liquid which is changed from semitransparent to full turbid and whitish;
(3) and (3) gel: the rising foam stops growing, a large number of bubbles are discharged from the surface of the foam, and the foam height stops changing after 100-700 s;
(4) curing: and (3) placing the gelled sponge in a shading and ventilating environment at the temperature of 30 ℃ for 5 days to obtain the required product.
The polyurethane sponges prepared in the above examples and comparative examples were subjected to related performance tests. The test method is as follows, and the test results are shown in table 2:
yellowing test: the ultraviolet radiation resistant polyurethane sponge prepared by the invention is put into an ultraviolet aging box for 24 hours. Generally, a laboratory simulation yellowing test judges color change by 1-5 levels, wherein 5 levels are unchanged, and the smaller the level number is, the poorer yellowing resistance is, namely the poorer ultraviolet resistance is.
And (3) testing the peel strength: the force applied when the sponge prepared by the invention is separated from the die by using a tensile machine under the same die is tested. The larger the test value, the worse the mold release ability.
Observation of the peeled surface: after demolding is completed, the sponge shape at the contact position of the sponge and the mold surface is observed by naked eyes.
Table 2 sponge property test results of examples and comparative examples
| Comparative example 1 | Comparative example 2 | Example 1 | Example 2 | Example 3 | Example 4 | |
| Yellowing test | 2 | 3.5 | 3.5 | 4 | 3 | 4.5 |
| Peel strength | 186 | 177 | 33 | 6 | 5 | 9 |
| Stripping surface | Incomplete | Incomplete | Is substantially complete | Smooth and complete | Smooth and complete | Smooth and complete |
The experimental results show that the polyurethane sponge prepared by the invention has better ultraviolet irradiation resistance and self-demolding capacity.
Claims (10)
1. The low-density ultraviolet radiation resistant polyurethane sponge comprises the following components in parts by weight:
2. the polyurethane sponge according to claim 1, wherein the polyether polyol is a low odor polyether polyol obtained by ring-opening polymerization of ethylene oxide and propylene oxide using glycerin and/or trimethylolpropane as an initiator; the unsaturation degree of the polyether polyol is less than 0.05mol/kg, the number average molecular weight is 3000-6000, and the molecular weight distribution is less than 1.05; wherein the content of the ethylene oxide in the mass of the polyether polyol is 5-30 wt% based on the total mass of the polyether polyol; the polyether polyol comprises one or more of F3135 of Wanhua chemical group, Inc., GEP-330N of high petrochemical, FA-703 of Coiya, EP-330NY of Shandong Lanxindong Daihong chemical Co Ltd, 3010 of DOW, F3156 of Wanhua chemical group, Inc., DEP-561D of Lanxindong Daoho, PPG-5623 of Shell brand and GEP-560s of high petrochemical, preferably F3156 and/or F3135 of Wanhua chemical group.
3. Polyurethane sponge according to claim 1 or 2, characterized in that the amine catalyst is selected from triethylenediamine and/or bis (dimethylaminoethyl) ether.
4. A polyurethane sponge according to any one of claims 1 to 3, wherein the organotin catalyst is stannous octoate and/or dibutyltin dilaurate.
5. The polyurethane sponge according to any one of claims 1 to 4, wherein the foam stabilizer is a silicone oil selected from one or more of the group consisting of silicone oils B8180, B8123, B8110, B8170.
6. A process for preparing a low density UV resistant polyurethane sponge according to any of claims 1 to 5, comprising the steps of:
(1) premixing: premixing 40-60% of dehydrated polyether polyol with the whole amount of tetrabutyl titanate and the whole amount of tributyl citrate, uniformly stirring, and taking the premix as a single component;
(2) stirring the milk white: mixing the premix with the rest components, stirring uniformly, and quickly pouring the mixture into a mold;
(3) and (3) gel: the rising foam stops growing, a large number of bubbles are discharged from the surface of the skin, and the foam height stops changing after a period of time;
(4) curing: and (3) placing the gelled sponge in a shading and ventilating environment for standing for a certain time to obtain the required product.
7. The process according to claim 6, wherein in step (1), the dehydrated polyether polyol has a water content of less than 200 ppm; the stirring time is 20-40 s.
8. The method according to claim 6, wherein in the step (2), the stirring time is 5-10 s.
9. The method according to claim 6, wherein in the step (3), the gel time is 100 to 700 s.
10. The method according to claim 6, wherein in the step (4), the curing temperature is 25-40 ℃ and the curing time is 1-9 days.
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| CN201910416311.9A CN111961184B (en) | 2019-05-20 | 2019-05-20 | Low-density ultraviolet radiation-resistant polyurethane sponge and preparation method thereof |
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| CN111961184B CN111961184B (en) | 2022-04-22 |
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| CN106366282A (en) * | 2016-09-21 | 2017-02-01 | 青岛德隆装备有限公司 | Polyurethane soft-hard foam combined forming process for beer barrel |
| CN108192322A (en) * | 2017-12-04 | 2018-06-22 | 张芸 | A kind of preparation method of hydrophobic oleophilic oil type polyurethane sponge |
| CN108559252A (en) * | 2017-12-19 | 2018-09-21 | 翟琳 | A kind of preparation method of railroad track resilient sleeper-bearing |
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