CN111072896A - Low-odor flame-retardant polyurethane foam material for vehicle interior decoration and preparation method thereof - Google Patents
Low-odor flame-retardant polyurethane foam material for vehicle interior decoration and preparation method thereof Download PDFInfo
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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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
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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
- C08G18/08—Processes
- C08G18/16—Catalysts
- C08G18/22—Catalysts containing metal compounds
- C08G18/225—Catalysts containing metal compounds of alkali or alkaline earth metals
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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
- C08G18/08—Processes
- C08G18/16—Catalysts
- C08G18/22—Catalysts containing metal compounds
- C08G18/24—Catalysts containing metal compounds of tin
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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
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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
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6461—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63 having phosphorus
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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
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- Polyurethanes Or Polyureas (AREA)
Abstract
The invention belongs to the field of polyurethane soft foam sponge materials, and particularly relates to a low-odor flame-retardant polyurethane foam material for vehicle interior decoration and a preparation method thereof, wherein the preparation method comprises the following steps: uniformly mixing low-odor polyol, high-purity water, low-odor flame-retardant silicone oil, a low-odor reactive flame retardant, an alkaline catalyst, a low-odor organic tin auxiliary agent and diisocyanate raw materials, foaming and forming by a one-step method, and cutting off top skins and side skins to cure for 1-3 days under the conditions of standard temperature and humidity to obtain the low-odor sponge. The sponge provided by the invention can meet the increasingly harsh odor requirement of a host factory on the automotive interior sponge on the premise of ensuring the flame retardance of the sponge.
Description
Technical Field
The invention belongs to the field of polyurethane soft foam sponge materials, and particularly relates to a low-odor flame-retardant polyurethane foam material for vehicle interior decoration and a preparation method thereof.
Technical Field
At present, the market has higher and higher requirements on the quality of air in a vehicle, and the requirements of a host factory on the sponge for interior decoration are also increasing. The taste of the sponge is mainly derived from: firstly, aldehydes generated by side reactions in the foaming process of polyether polyol, such as formaldehyde, acetaldehyde and acrolein; secondly, the odor substances of micromolecule styrene and acrylonitrile introduced by polymer polyol; thirdly, amine odor derived from amine emission; fourthly, the emission of the additive liquid flame retardant is obtained; the raw materials can influence the smell of the sponge in different degrees, and the raw materials are further developed along with the continuous progress of raw material technology, for example, the use of a new catalyst can reduce the unsaturation degree of polyether to an extremely low level, the new process can greatly reduce the smell of silicone oil, the new technology can enable the catalyst to have complete reaction activity, the amine smell in the sponge is completely eradicated by the novel alkaline catalyst, and the automotive interior flame-retardant sponge can meet the requirement of a host factory on the smell of the sponge by matching with a proper curing process on the premise of meeting the flame retardance.
The patent application No. CN201410855589.3 describes that the odor of the sponge is reduced by selecting a reactive flame retardant and adding MC, but compared with the sponge related to the patent, the patent does not make preference for polyether and a catalyst, and actually the quality of the polyether and the amine catalyst also have extremely important influence on the odor of the sponge; the application number CN201510026241.8 patent describes a preparation method of low-odor polyurethane elastomer, the material involved in the patent is foaming sponge, which is not the same type of material, wherein, a porous structure substance deodorant is required to be added, so as to reduce the volatilization amount of organic molecules; the patent application No. CN201510207744.5 describes a preparation method of low-odor rigid polyurethane foam. Firstly, hard bubbles are prepared, the materials involved in the patent are soft bubbles and are not the same type of materials; wherein more expensive catalysts are required to be compounded for use to meet the performance requirements. Patent application No. CN201610807857.3 describes a preparation method of a molded foam, non-flame-retardant low-odor sponge, and the material involved in the patent is a flame-retardant horizontal foam which is continuously produced, has different processes and functionalities, and still needs to be added with an amine catalyst; the patent application numbers CN201810037318.5 and 201811039383.8 describe a preparation method of low-odor polyurethane semi-hard foam, the material involved in the patent is soft foam, the requirements on the performance of the material are different, and hydrazine hydrate is added, so that the odor is large; application No. CN201810755044.3 describes a preparation method of low-odor high-resilience polyurethane foam, which is different from the performance requirements of the present invention for materials, wherein an aldehyde scavenger is required to be added, and expensive amine is used for catalysis; and CN201811039382.3 patent, which is different from the present invention in terms of material performance requirements, and expensive amine catalysis.
After analyzing the existing prior art, the inventor finds that although the odor problem is more and more concerned in the preparation of polyurethane materials in the field, the odor problem is solved differently, some are to add special porous materials to reduce the volatilization of organic molecules, and some are to add aldehyde scavengers, etc. Most solutions to this problem have centered around the control of the odor of the raw materials. Although the use of low-odor raw materials and auxiliary agents, which are known to those skilled in the art and whose reaction yields materials with reduced odor, has to be faced with a more serious problem in the course of this development. That is how to ensure the mechanical properties of the material itself. Among polyurethane materials, organic amine catalysts are most widely used because of their remarkable efficacy in foaming reactions and their synergistic effect with organotin catalysts. Therefore, the amine-based catalyst is not separated from the prepared polyurethane material. Although in the above prior art some low odor amine catalysts are used, this necessarily increases the production costs.
Therefore, how to avoid using any amine catalyst and to stop the amine smell in the sponge, the sponge obtained after horizontal foaming can not only meet the latest requirements of host factories on the smell of the decorative sponge, but also ensure the flame retardant and mechanical properties thereof by the preferable selection of raw materials and the re-selection and compounding of the catalyst, and the problem which needs to be solved at present is urgently needed.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a low-odor flame-retardant polyurethane foam material for automotive interiors and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical means:
uniformly mixing low-odor polyol, high-purity water, low-odor flame-retardant silicone oil, a low-odor reactive flame retardant, an alkaline catalyst, a low-odor organic tin auxiliary agent and diisocyanate, mixing in a high-pressure or low-pressure machine, foaming and forming by a one-step method, cutting off the top skin and the side skin and curing for 1-3 days under the condition of standard temperature and humidity, and thus obtaining the low-odor flame-retardant sponge for the vehicle. The sponge prepared by the invention can meet the harsh odor requirement of a host factory on the automotive interior sponge.
The low-odor flame-retardant polyurethane foam comprises the following raw materials in parts by weight: 90-120 parts of low-odor polyether polyol, 2-4 parts of pure water, 0.2-5 parts of low-odor flame-retardant silicone oil, 5-10 parts of low-odor reaction type flame retardant, 1-3 parts of alkaline catalyst, 0.01-0.15 part of low-odor organic tin auxiliary agent and 40-100 parts of diisocyanate.
The foaming agent is water, the water reacts with isocyanate to generate gas carbon dioxide, so that the foam body expands and foams, and the using amount of the water ranges from 2 parts to 4 parts.
Wherein, the low-odor polyether polyol is polyol with highly concentrated molecular weight, which is prepared by removing small molecules through nitrogen blowing vacuum and adopting a catalyst; a functionality of 2 to 4 and a hydroxyl value of 100 to 500 mgKOH/g.
The low-odor polyether polyol is one or a mixture of more of polyether polyol with the molecular weight of 3000-12000 and polytetrahydrofuran ether type polyol
Preferably, the low-odor polyether polyol is available in one or more of the market designations MD-4618 (purchaser: Singapore Shell), HS-100 (purchaser: Bayer), LHS-200 (purchaser: Shandong Longhua), SC-5616S (purchaser: Zhonghai Shell).
The low-odor flame-retardant silicone oil is flame-retardant silicone oil with small molecules removed in vacuum, and the production process and equipment are specially designed to be different from conventional silicone oil and can effectively and uniformly disperse foaming raw materials; preferably, the low-odor flame-retardant silicone oil is one or a mixture of RZ-8960 (a purchasing manufacturer such as a sharp-rank new material), B-8244 (a purchasing manufacturer such as winning), L-5702, L-650(L-5702, a purchasing manufacturer of L-650 flame-retardant silicone oil such as Mylar chart) and BL-820LF (a purchasing manufacturer: Maihao chemical industry).
The basic catalyst is different from amine catalysts used in the polyurethane soft foam industry, comprises an additive amine catalyst and a reactive amine catalyst, and is the biggest difference of the formula process of the invention from the soft foam industry; preferably, the basic catalyst is one or more of alkali metal salts such as sodium carbonate, sodium bicarbonate, sodium hydroxide, sodium chloride, potassium chloride, etc., and amine smell in the sponge is completely eliminated.
The low-odor organic tin catalyst refers to low odor such as stannous octoate and dibutyltin dilaurate, and preferably, the market brand of the low-odor organic tin catalyst is one or a mixture of DBTDL-19 (D-19, a purchaser such as a cis-promoter in Guangzhou Zengcheng), DBTDL-25, T-9 (stannous isooctanoate, a purchaser such as Shanghai ran chemical Co., Ltd.), and T12 (dibutyltin dilaurate (T-12), a purchaser such as American Aikoku, Shanghai De Xuan chemical Co., Ltd.).
Wherein the low-odor reaction type flame retardant can be a powdery phosphate polymer or a liquid phosphate polymer, the phosphorus content is more than 5 percent, and the hydroxyl value is not less than 50 mgKOH/g; preferably, the market brands of the flame retardant are RZ-886 (New Ruizhenya material), YK-7HF and YK-115 (Xianyangya), HC-1020 (Korean Innovative material);
the diisocyanate is one or more of TDI, MDI, PAPI, IPDI and HMDI, comprises a modified polymer of the diisocyanate, and has NCO content of 12-48%, and preferably the market trademark of the diisocyanate is one or more of TDI-80, MDI-3133 and MDI-6510.
The preparation method of the polyurethane foam material comprises the following steps:
and uniformly mixing and foaming the materials, and curing after foaming to obtain a polyurethane sponge finished product.
The foaming mode is as follows: foaming can be carried out by adopting a horizontal foaming machine, a vertical foaming machine, box foaming and the like. Including high pressure or low pressure mixing. Wherein, a horizontal foaming machine is used, the stirring speed of a mixing head is 4000-5000 r/min, and the pressure is 5-8 Mpa.
Preferably, the standard chamber temperature at the time of foaming is 25 ℃; the material temperature is 23-25 ℃; the relative humidity of the foaming environment is 50%, and the foaming speed is 3-5 m/min.
Curing: and (3) obtaining a polyurethane latex foam body after foaming, cutting off the top skin and the side skin and curing for 1-3 days under the condition of standard humidity, thus obtaining a polyurethane sponge finished product. The curing temperature is room temperature, and the relative humidity of the curing environment is 50%.
Compared with the prior art, the invention has the beneficial effects that:
the invention selects the alkaline catalyst and the low-odor organic tin catalyst to be compounded for use, wherein the alkaline catalyst (preferably sodium carbonate and sodium hydroxide) is alkaline and can promote the addition polymerization of polyurethane, and the alkaline catalyst has the advantages that: 1. the raw materials are wide in source and low in price, and the production cost is obviously reduced; 2. the catalyst is compounded with an organic tin catalyst for use, and can effectively promote the reaction of the polyol and the isocyanate to form a polymer. 3. The reaction rate of water and isocyanate is accelerated, so that the foaming opening rate is increased; 4. the alkaline catalyst is different from an amine catalyst, so that the odor of amine is completely eradicated, and the normal foaming can be realized only by simultaneously adjusting raw materials and a process, so that the odor of amine in a system is eradicated, and the requirement of low odor is met. And the cellular structure can be 100PPI from 5PPI, so that the requirements of air permeability and comfort are met.
Detailed Description
The following are specific examples of the present invention and further description of the technical solutions of the present invention, and these examples are only used for illustrating the present invention and are not used to limit the protection scope of the present invention. In practice, the invention will be understood to cover all modifications and variations of this invention provided they come within the scope of the appended claims.
The relative humidity of the foaming environment is 50%, the temperature is 25 ℃, and the material temperature is 23-25 ℃.
Example 1
The low-odor flame-retardant polyurethane foam material is prepared from the following raw materials in parts by weight:
110 parts of low-odor polyether polyol (wherein the parts are MD-4618100 parts and HS-10010 parts), 2.8 parts of pure water and an alkaline catalyst (NaCO)3) 1.2 parts of low-odor organic tin auxiliary agent (D-19), 0.11 part of low-odor flame-retardant silicone oil (B-8244), 7 parts of low-odor reaction type flame retardant (YK-7HF) and 42 parts of diisocyanate (TDI-80).
Uniformly mixing and foaming the raw materials at room temperature (horizontal foaming), stirring at 4300rpm, the pressure of 53bar and the foaming speed of 3-5 m/min to form a strip foam or a block foam sponge, cutting off the top skin and the side skin, and curing at room temperature for 2 days to obtain the low-odor flame-retardant polyurethane foam material.
Example 2
The low-odor flame-retardant polyurethane foam material is prepared from the following raw materials in parts by weight:
100 parts of low-odor polyether polyol (wherein the parts are MD-461890 parts and HS-10010 parts), 3.6 parts of pure water and an alkaline catalyst (NaCO)3) 1.4 parts of low-odor organic tin auxiliary agent (D-19), 1.1 parts of low-odor flame-retardant silicone oil (RZ-8960), 8 parts of low-odor reaction type flame retardant (RZ-886) and 51.8 parts of diisocyanate (TDI-80).
Uniformly mixing and foaming the raw materials at room temperature (horizontal foaming), stirring at 4000rpm, under 62bar, and at a foaming speed of 3-5 m/min to form a strip foam or a block foam sponge, cutting off the top skin and the side skin, and curing at room temperature for 2 days to obtain the low-odor flame-retardant polyurethane foam material.
Example 3
The low-odor flame-retardant polyurethane foam material is prepared from the following raw materials in parts by weight:
100 parts of low-odor polyether polyol (MD-4618), 2.5 parts of pure water and an alkaline catalyst (NaCO)3) 1.55 parts of low-odor organic tin auxiliary agent (D-19)0.03 parts of low-odor flame-retardant silicone oil (L-5702) 0.8 parts of low-odor reaction type flame retardant agent (RZ-886)6 parts of low-odor reaction type flame retardant agent (MDI-6510)) 55 parts of low-odor reaction type flame retardant agent (MDI-6510).
Uniformly mixing and foaming the raw materials at room temperature, stirring at the rotating speed of 4500rpm, the pressure of 68bar, and the foaming speed of 3-5 m/min to form strip foam or block foam sponge, cutting off the top skin and the side skin, and curing at room temperature for 2 days to obtain the low-odor flame-retardant polyurethane foam material.
The polyurethane foams prepared in examples 1 to 3 were subjected to property tests, and the test results are shown in Table 1.
Table 1:
as can be seen from Table 1, the invention selects the types of raw materials and limits the mass relationship among the components, so that the components can generate excellent synergistic action, no amine catalyst is used in the finally prepared flame-retardant polyurethane foam material, the foamed sponge can still meet the requirements of mechanics and flame retardance, the grade of PV3900-2000 is lower than 3, and the latest requirements of host factories on the odor of decorative sponges are fully met.
Comparative example 1
Comparative example 1 compared with example 1, the raw materials are the same, and the main difference is that the preparation method is different.
The raw materials are uniformly mixed and foamed (horizontally foamed) at room temperature, the stirring speed is 2000rpm, the pressure is 40bar, the foaming reaction effect is poor, the polyurethane with expected mechanical properties is difficult to foam, the breaking elongation is 80%, and the tensile strength is 60 KPa.
Comparative example 2
Comparative example 2 compared to example 1, the process was the same, the main difference being that NaCO was used3The catalyst was replaced with the lower odor amine catalyst triethylenediamine. The prepared polyurethane sponge achieves the expected effect on the mechanical property, but the odor grade of PV3900-2000 is 4.5, and compared with the invention, the odor requirement of the invention is difficult to achieve.
Comparative example 3
Comparative example 3 compared to example 1, the process was the same, the main difference being that NaCO3The amount of the catalyst used was 0.5 part, and the other conditions were the same. The polyurethane has poor foaming pore diameter effect, and the elongation at break and the tensile strength are both seriously reduced and are respectively 90 percent and 69 KPa.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified. The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all modifications of the above embodiments made according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A low-odor flame-retardant polyurethane foam material for vehicle interior decoration is characterized in that: the material comprises the following raw materials in parts by weight: 90-120 parts of low-odor polyether polyol, 2-4 parts of pure water, 0.2-5 parts of low-odor flame-retardant silicone oil, 5-10 parts of low-odor reaction type flame retardant, 1-3 parts of alkaline catalyst, 0.01-0.15 part of low-odor organic tin auxiliary agent and 40-100 parts of diisocyanate.
2. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the low-odor polyether polyol is polyether polyol with the molecular weight of 3000-12000, the functionality of 2-3 and one or more of polytetrahydrofuran ether type polyol.
3. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the low-odor polyether polyol is one or a mixture of MD-4618, HS-100, LHS-200 and SC-5616S.
4. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the low-odor flame-retardant silicone oil is one or a mixture of RZ-8960, B-8244, L-5702, L-650 and BL-820 LF.
5. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the low-odor reaction type flame retardant is a powdery phosphate polymer or a liquid phosphate polymer, the phosphorus content is more than 5 percent, and the hydroxyl value is not lower than 50 mgKOH/g.
6. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the alkaline catalyst is one or a mixture of sodium carbonate, sodium hydroxide, sodium bicarbonate, sodium chloride and potassium chloride.
7. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the low-odor organic tin auxiliary agent is as follows: stannous octoate or dibutyltin dilaurate.
8. The low-odor flame-retardant polyurethane foam for vehicle interior according to claim 1, characterized in that: the diisocyanate is one or more of TDI, MDI, PAPI, IPDI and HMDI or a modified polymer of diisocyanate; the NCO content is 12-48%.
9. The preparation method of the low-odor flame-retardant polyurethane foam material for interior trims of vehicles according to any one of claims 1 to 8, which comprises the following specific preparation steps:
(1) uniformly mixing low-odor polyhydric alcohol, water, low-odor flame-retardant silicone oil, a low-odor reaction type flame retardant, an alkaline catalyst, a low-odor organic tin auxiliary agent and diisocyanate, and foaming and molding by adopting a high-pressure or low-pressure foaming machine in a one-step method;
(2) and cutting off the top skin and the side skin of the foamed polyurethane sponge, and curing for 1-3 days to obtain the low-odor sponge.
10. The method for preparing a low-odor flame-retardant polyurethane foam material for interior trims of vehicles according to claim 9, wherein: the stirring speed of the high-pressure foaming machine is 4000-; the foaming environment has a relative humidity of 50% and a temperature of 25 ℃.
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| CN116789925A (en) * | 2023-07-07 | 2023-09-22 | 江苏米尔化工科技有限公司 | Formaldehyde-free low-odor polyurethane foam material and preparation method thereof |
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