CN116333260A - Full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and preparation method thereof - Google Patents

Full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and preparation method thereof Download PDF

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CN116333260A
CN116333260A CN202310128968.1A CN202310128968A CN116333260A CN 116333260 A CN116333260 A CN 116333260A CN 202310128968 A CN202310128968 A CN 202310128968A CN 116333260 A CN116333260 A CN 116333260A
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chain extender
damping material
polyurethane
catalyst
foaming
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瞿金磊
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Qingdao Haishengtai Material Co ltd
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Qingdao Haishengtai Material Co ltd
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Abstract

The invention relates to the field of functional material manufacturing, and particularly provides a full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and a preparation method thereof. The micropore damping material is prepared from the following components: 70-100 parts by weight of polyurethane prepolymer, 5-50 parts by weight of suspension chain extender and foaming homogenizing agent combination; the polyurethane prepolymer is obtained by reacting polyester dihydric alcohol and diisocyanate; the suspension chain extender is obtained by reacting polyethylene glycol monomethyl ether and diisocyanate under the action of a catalyst; the microporous elastomer is obtained through strong stirring, mould pressing, foaming and post curing. The dual-peak temperature of the damping material is about-30 to-25 ℃ and 30 to 40 ℃, the foaming pore diameter distribution is 50 to 180 mu m, the high and low temperatures are matched with the using temperature range of the household appliance, and the damping material has good application prospect.

Description

Full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and preparation method thereof
Technical Field
The invention relates to the field of functional material manufacturing, and particularly provides a full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and a preparation method thereof.
Background
With the development of society, mechanical equipment tends to be high-speed, efficient and automatic, but vibration, noise and fatigue fracture caused by the development of society are also more and more prominent, and the vibration and the noise limit the improvement of the performance of the mechanical equipment, seriously damage the stability and the reliability of the operation of the mechanical equipment, pollute the environment and harm the physical and mental health of people.
For this reason, various methods and technical measures for solving the vibration and noise problems in engineering have been studied and developed, wherein the damping technology is the most effective method for controlling the resonance and noise of the structure, and is the most important means for solving the vibration and noise reduction problems. However, the effective damping of the traditional damping material is single-peak damping, the damping temperature is in a low temperature region, and the requirement of self-adaptive damping performance adjustment of equipment cannot be met.
The polyurethane material synthesis has the advantages of controllability, strong designability, diversified foaming performance and the like, becomes one of research hot spots of the microporous elastomer damping material, but the polyurethane damping material has the same defects of the viscoelastic damping material, namely good damping performance below room temperature and poor damping effect above room temperature, so the polyurethane elastomer damping material needs to be structurally designed, the polyurethane elastomer consists of soft and hard segments, the designability is strong, the free volume fraction (the percentage of free volume holes to the total volume of the polymer) is reasonable, the compatibility of the soft and hard segments of the polyurethane elastomer is regulated by introducing a suspension chain and the like, microphase separation is improved, and the material with good damping performance in a wide temperature range or a multi-temperature range can be prepared, so the application field and the range of the polyurethane damping material are further widened.
Disclosure of Invention
Based on the reasons, the invention provides a full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and a preparation method thereof. The invention introduces a side chain structure with certain molecular weight through molecular structure design, and overcomes the defect that a single damping product cannot meet the actual use requirement. The damping material is obtained after strong stirring, mould pressing, foaming and post curing, has high tensile strength performance, excellent pressure resistance and change performance, good wear resistance, bimodal damping temperature of minus 30 ℃ to minus 25 ℃ and 30 ℃ to 40 ℃ respectively, foam pore size distribution of 50 mu m to 180 mu m, high and low temperature matching with the using temperature range of household appliances, and has good application prospect.
The specific technical scheme of the invention is as follows:
the polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: 70-100 parts of polyurethane prepolymer, 5-50 parts of suspension chain extender and foaming chain extender composition.
Wherein the polyurethane prepolymer is prepared by reacting polyester diol and diisocyanate according to the prior conventional technology, and the weight ratio of the polyester diol to the diisocyanate is (70-100): (20-40).
The polyester diol is conventionally selected, but preferably one or more of polycaprolactone polyol, polyethylene adipate and polybutylene adipate are mixed. More preferably, the molecular weight of the polyester diol is 1000-2000, preferably 2000, and the water content after dehydration under vacuum of-0.096 to-1 MPa can be lower than 0.5 per mill.
The diisocyanate is conventionally selected, but is preferably selected from the group consisting of 2, 4-toluene diisocyanate (TDI-100), and Naphthalene Diisocyanate (NDI).
The suspension chain extender and the foaming chain extender composition thereof are a combination of the suspension chain extender, small molecular dihydric alcohol, a catalyst, a foam homogenizing emulsifier and a foaming agent, and the suspension chain extender is prepared from the following components in percentage by weight: small molecule diols: catalyst: homogenizing emulsifying agent: the foaming agent is 18-22:3-6:0.2-0.4:6-9:4-6.
The catalyst is a combination catalyst of organic tin and triethylenediamine, and the weight ratio of the organic tin to the triethylenediamine is preferably 1:2, wherein the organic tin can be selected from stannous octoate or/and dibutyl tin dilaurate, and the dibutyl tin dilaurate is preferred. The catalyst is used for regulating and controlling the reaction speed of foaming and gel, improving the speed of foaming, chain extension and crosslinking, realizing the matching of the speed of foaming and gel and improving the production efficiency.
The suspension chain extender is obtained by reacting polyethylene glycol monomethyl ether and diisocyanate under the action of an organotin catalyst, wherein the molecular weight of the polyethylene glycol monomethyl ether is 1000-2000; the diisocyanate is isophorone diisocyanate; the organotin catalyst may be of a kind conventional in the art, such as dibutyltin dilaurate T12 or stannous octoate T9; the consumption of the organotin catalyst is preferably 1 to 5 per mill of the total mass of the polyethylene glycol monomethyl ether and the diisocyanate; the preferred molar ratio of polyethylene glycol monomethyl ether to diisocyanate is 1:1.
The suspension chain extender is prepared according to a conventional method, and the specific preparation process is preferably as follows: under the condition of inert gas protection and medium-speed stirring, mixing polyethylene glycol monomethyl ether and diisocyanate, heating to 50 ℃, adding an organotin catalyst, and reacting for 2 hours to stop the reaction, thus obtaining a suspension chain extender; the inert gas is N 2 The method comprises the steps of carrying out a first treatment on the surface of the The molecular weight of polyethylene glycol monomethyl ether in the suspension chain extender is 1000-2000, which determines the peak height of one of the double damping peaks of the polyurethane microporous elastomer material in the invention, namely the damping performance, and the invention is applied to the technical proposalPlays a key role; while the diisocyanate is chosen from isophorone diisocyanate, depending on which on the one hand provides reactive groups with the polyester polyol to prepare the prepolymer and on the other hand provides reactive groups for foaming chain extension crosslinking, the inventive materials can be prepared.
The small molecular dihydric alcohol can be one or two of the conventional selected types, preferably ethylene glycol, propylene glycol, diethylene glycol and 1, 4-butanediol, and the mixing ratio is 1:1 when the small molecular dihydric alcohol is mixed for use.
The foam homogenizing emulsifier is preferably a mixture of alkylphenol ethoxylates OP-10, sorbitan monooleate-80 and polysorbate-80 in a weight ratio of 3:1:1. According to the invention, the composite foam homogenizing emulsifier is selected, so that on one hand, the polar components (such as water) and the nonpolar components in the reaction system can be more fully and uniformly dispersed; more importantly, the compounded foam homogenizing emulsifier plays an important role in regulating and controlling the size of the foam holes of the polyurethane microporous elastomer material, and other types or single components or mixtures with different proportions can have poor effects. The total amount of the foam homogenizing emulsifier is 1.5 times that of the foaming agent.
The foaming agent is water, preferably high-purity water or ultrapure water, the conductivity is less than 0.1 mu s/cm and the residual salt content is less than 0.3mg/L at 25 ℃, and the water with non-dielectric trace bacteria, microorganisms, particles and other impurities removed is used for preventing the influence of mineral and other impurities on the foaming reaction and the storage of materials, and the proportion is 0.5-2% of the polyurethane prepolymer.
The preparation method of the polyurethane microporous elastomer double-peak damping material comprises the following specific steps:
(1) Preparation of polyurethane prepolymers
Heating the polyester diol to 100-120 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; under the protection of inert gas and medium-speed stirring, mixing dehydrated polyester diol and diisocyanate, heating to 70-80 ℃, and stopping the reaction after heat preservation for 1-3 hours to obtain an elastic main chain prepolymer, namely polyurethane prepolymer; the inert gas is N 2 。
(2) Suspension chain extender and preparation of foaming chain extender composition thereof
And (3) carrying out vacuum degassing on the suspension chain extender, the micromolecular dihydric alcohol, the catalyst and the homogenizing emulsifier until no bubble exists, uniformly mixing the suspension chain extender with the foaming agent, and carrying out high-power emulsification on the suspension chain extender for 1 hour for standby.
(3) Preparation of polyurethane microporous elastomer damping material
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 65-90 ℃ according to a proportion, rapidly stirring, heating to 90-95 ℃, preserving heat for 0.5-2h, curing, continuously heating to 100-150 ℃, preserving heat for 10-26 h, and curing to obtain the microporous polyurethane elastomer damping material.
The damping performance of the polyurethane microporous elastomer double-peak damping material is characterized by a double-peak structure, the corresponding temperatures of damping peaks are-30 to-25 ℃ and 30 to 40 ℃, and the size distribution of cells is 50 to 180 mu m. The two damping peaks of the material are mainly based on the special molecular design of the invention, so that the material has two chain structures of a main side chain, and corresponding damping peaks are respectively generated. The key to introducing side chains to create two damping peaks is that the molecular weight of the side chains, when below a critical value, is insufficient to create sufficient relaxation hysteresis, the bimodal character cannot be seen. When the molecular weight is large to a certain value, hysteresis is generated due to energy consumption such as entanglement with a main chain, hydrogen bond dissociation recombination and internal friction in the movement process, and a second damping peak is generated. The molecular weight of the side chain polyethylene glycol monomethyl ether determines the peak height of one of the dual damping peaks, i.e., the damping performance. According to the invention, through research design, a proper suspension chain extender and a foaming chain extender composition thereof are selected, and combined with polyurethane prepolymer (especially after the molecular weight of polyester diol is limited), the polyurethane microporous elastomer material with the bimodal damping characteristic is obtained, and the bimodal corresponding temperature can meet the requirements of multiple fields, so that the polyurethane microporous elastomer material is particularly suitable for the field of household appliances.
In conclusion, the full-water foaming polyurethane microporous elastomer double-peak damping material based on the molecular structure design provided by the invention has good mechanical strength, rebound resilience and thermal stability, particularly has a uniformly distributed cell structure and double damping peaks, and has great progress compared with the existing product in wide application range.
Drawings
FIG. 1 is a graph of loss factor tan delta versus temperature for the material of example 6;
FIG. 2 is a graph of loss factor tan delta versus temperature for the material of comparative example 1;
FIG. 3 is a scanning electron microscope comparison chart of the materials of example 5 and comparative example 2.
Detailed Description
The above-described aspects of the present invention will be described in further detail by way of the following embodiments, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples. All techniques implemented based on the above description of the invention are within the scope of the invention. The following examples were carried out using conventional techniques, except as specifically described.
Example 1
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: 70 parts of polycaprolactone diol/TDI-100 prepolymer, 10 parts of suspension chain extender and 10 parts of foaming chain extender composition.
The preparation process comprises the following steps:
heating polycaprolactone diol to 120 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And under the protection and medium-speed stirring, mixing dehydrated polycaprolactone dihydric alcohol (molecular weight 2000)/TDI-100 according to the proportion of 100:30, heating to 70 ℃, and stopping the reaction after heat preservation for 1h to obtain the elastic main chain prepolymer, namely the polyurethane prepolymer.
Under the condition of inert gas N 2 Under the conditions of protection and stirring, mixing 2000 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate according to a molar ratio of 1:1, heating to 50 ℃, adding 2 per mill (based on the total mass of the reaction raw material mixture) of a T9 catalyst, and stopping the reaction for 2 hours to obtain the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to the weight ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, the ethylene glycol, the catalyst and the homogenizing emulsifier are mixed with foaming agent water uniformly after being degassed in vacuum until no bubbles exist, and the mixture is emulsified for 1 hour on an emulsifying machine for standby in a high power way, wherein the ratio of the suspension chain extender to the ethylene glycol to the catalyst to the homogenizing emulsifier to the water is 20:5:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding a chain extender and a foaming chain extension composition into the polyurethane prepolymer at 75 ℃, rapidly stirring, heating to 90 ℃, preserving heat for 0.5h, curing, continuously heating to 120 ℃, preserving heat for 12h, and curing to obtain the polyurethane elastomer damping material.
The damping material obtained in the embodiment has a damping performance characteristic of a double-peak structure, the corresponding temperatures of damping peaks are minus 28 ℃ and 36 ℃, and the size distribution of cells is 50-150 mu m.
Example 2
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: 80 parts of polycaprolactone diol/TDI-100 prepolymer, 13.1 parts of suspension chain extender and 13.1 parts of foaming chain extender composition.
The preparation process comprises the following steps:
heating polycaprolactone diol to 105 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And under the protection and medium-speed stirring, mixing dehydrated polycaprolactone diol/TDI-100 with the molecular weight of 2000 according to the proportion of 100:29, heating to 75 ℃, and stopping the reaction after heat preservation for 2 hours to obtain the elastic main chain prepolymer, namely the polyurethane prepolymer.
In an inert gas N 2 Under the conditions of protection and stirring, mixing polyethylene glycol monomethyl ether with the molecular weight of 2000 and isophorone isocyanate according to the molar ratio of 1:1, heating to 50 ℃, adding 1%o of T12 catalyst (according to the total mass of the reaction raw material mixture), and stopping the reaction for 2 hours to obtain the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to a ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, propylene glycol, catalyst and homogenizing emulsifier are mixed with foaming agent water after vacuum degassing until no bubble exists, and the mixture is emulsified for 1 hour on an emulsifying machine for standby under high power, wherein the suspension chain extender and propylene glycol are as follows: catalyst: the ratio of the foam homogenizing emulsifying agent to the water is 20:7.5:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 90 ℃ according to the formula proportion, rapidly stirring, heating to 95 ℃, preserving heat for 1h, continuously heating to 110 ℃ after curing, preserving heat for 26h, and curing to obtain the polyurethane elastomer damping material.
The damping performance of the damping material obtained in the embodiment is characterized by a double-peak structure, the corresponding temperatures of damping peaks are-29 ℃ and 35 ℃, and the size distribution of the cells is 50-140 mu m.
Example 3
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: polycaprolactone diol/TDI-100 prepolymer 100, hanging chain extender foaming chain extender composition 13.8.
The preparation process comprises the following steps:
heating polycaprolactone diol to 100 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And under the protection and medium-speed stirring, mixing dehydrated polycaprolactone diol with 2000 molecular weight and TDI-100 diisocyanate according to the proportion of 100:27, heating to 70-80 ℃, preserving heat for 2.5h, and stopping reacting to obtain the elastic main chain prepolymer, namely the polyurethane prepolymer.
In an inert gas N 2 Under the conditions of protection and stirring, mixing 2000 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate according to a molar ratio of 1:1, heating to 50 ℃, adding 1%o of T12 catalyst (based on the total mass of the reaction raw material mixture), and stopping the reaction for 2 hours to obtain the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to a ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, the 1, 4-butanediol, the catalyst and the homogenizing emulsifier are subjected to vacuum degassing until no bubble exists, and then are uniformly mixed with foaming agent water, and are emulsified on an emulsifying machine for 1 hour under high power for standby, wherein the suspension chain extender and the 1, 4-butanediol are prepared by the following steps: catalyst: the ratio of the foam homogenizing emulsifying agent to the water is 20:7.5:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 85 ℃ according to the formula proportion, rapidly stirring, heating to 91 ℃, preserving heat for 2 hours, continuously heating to 130 ℃ after curing, preserving heat for 13 hours, and curing to obtain the polyurethane elastomer damping material.
The damping material obtained in the embodiment has a damping performance characteristic of a double-peak structure, the corresponding temperatures of damping peaks are minus 28 ℃ and 36 ℃, and the size distribution of cells is 50-150 mu m.
Example 4
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: polybutylene adipate/TDI-100 prepolymer 100, catenary chain extender and foaming chain extender composition 13.8.
The preparation process comprises the following steps: heating polybutylene adipate to 100 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And under the protection and medium-speed stirring, mixing dehydrated polybutylene adipate (molecular weight 2000) with TDI-100 according to a ratio of 100:27, heating to 80 ℃, and stopping the heat preservation reaction for 1 hour to obtain the elastic main chain prepolymer, namely the polyurethane prepolymer.
In an inert gas N 2 Under the conditions of protection and stirring, mixing 2000 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate according to a molar ratio of 1:1, heating to 50 ℃, adding a T12 catalyst of 3 per mill, and stopping the reaction for 2 hours to obtain the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to a ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, the 1, 4-butanediol, the catalyst and the homogenizing emulsifier are subjected to vacuum degassing until no bubble exists, and then are uniformly mixed with foaming agent water, and are emulsified on an emulsifying machine for 1 hour under high power for standby, wherein the suspension chain extender, the propylene glycol and the 1, 4-butanediol are prepared by the steps of: catalyst: the ratio of the foam homogenizing emulsifying agent to the water is 20:3.75:3.75:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 75 ℃ according to the formula proportion, rapidly stirring, heating to 90 ℃, preserving heat for 0.5h, continuously heating to 100 ℃ after curing, preserving heat for 16h, and curing to obtain the polyurethane elastomer damping material.
The damping material obtained in the embodiment has a damping performance characteristic of a double-peak structure, the corresponding temperatures of damping peaks are minus 28 ℃ and 35 ℃, and the size distribution of cells is 55-145 mu m.
Example 5
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: polycaprolactone diol/TDI-100 prepolymer 100, catenary chain extender, and foaming chain extender composition 13.8.
The preparation process comprises the following steps: heating polycaprolactone diol to 110 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And under the protection and medium-speed stirring, mixing dehydrated polycaprolactone diol with 2000 molecular weight and TDI100 diisocyanate according to a ratio of 100:27, heating to 75 ℃, and stopping the reaction after heat preservation for 1h to obtain an elastic main chain prepolymer, namely a polyurethane prepolymer.
Under the protection of inert gas and stirring, mixing 2000 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate according to a molar ratio of 1:1, heating to 50 ℃, adding 4%o of T12 catalyst (based on the total mass of the reaction raw material mixture), and stopping the reaction for 2 hours to obtain the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to a ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, the 1, 4-butanediol, the catalyst and the homogenizing emulsifier are subjected to vacuum degassing until no bubble exists, and then are uniformly mixed with foaming agent water, and are emulsified on an emulsifying machine for 1 hour under high power for standby, wherein the suspension chain extender, the propylene glycol and the 1, 4-butanediol are prepared by the steps of: catalyst: the ratio of the foam homogenizing emulsifying agent to the water is 20:3.75:3.75:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding a chain extender and a foaming chain extension composition into the polyurethane prepolymer at 72 ℃ according to the formula proportion, rapidly stirring, heating to 95 ℃, preserving heat for 0.5h, curing, continuously heating to 120 ℃, preserving heat for 18h, and curing to obtain the polyurethane elastomer damping material.
The damping material obtained in the embodiment has a damping performance characteristic of a double-peak structure, the corresponding temperatures of damping peaks are-27 ℃ and 35 ℃, and the size distribution of cells is 60-150 mu m.
Example 6
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: polycaprolactone diol/NDI prepolymer 90, catenary chain extender, and foaming chain extender composition 12.5.
The preparation process comprises the following steps: heating polycaprolactone diol to 100 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And mixing the dehydrated polycaprolactone diol with the molecular weight of 2000 with NDI diisocyanate according to the ratio of 100:33 under the conditions of protection and medium-speed stirring, heating to 75 ℃, and stopping the reaction after the heat preservation is carried out for 3 hours to obtain the elastic main chain prepolymer, namely the polyurethane prepolymer.
In an inert gas N 2 Under the conditions of protection and stirring, 2000 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate are mixed according to a molar ratio of 1:1, the temperature is raised to 50 ℃, and a T12 catalyst with the total mass of 5 per mill of the reaction raw material mixture is addedAnd stopping the reaction after 2 hours of reaction to obtain the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to a ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, 1, 4-butanediol, a catalyst and a homogenizing emulsifier are subjected to vacuum degassing until no bubble exists, and then are uniformly mixed with foaming agent water, and are emulsified on an emulsifying machine for 1 hour under high power for standby, wherein the suspension chain extender is prepared by the following steps: 1, 4-butanediol: catalyst: homogenizing emulsifying agent: the water ratio was 20:7:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 65 ℃ according to the formula proportion, rapidly stirring, heating to 90 ℃, preserving heat for 0.5h, curing, continuously heating to 120 ℃, preserving heat for 16h, and curing to obtain the polyurethane elastomer damping material.
The damping performance of the damping material obtained in the embodiment is characterized by a double-peak structure, the corresponding temperatures of damping peaks are minus 26 ℃ and 33 ℃, and the size distribution of the cells is 80-180 mu m.
Comparative example 1
The polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: polycaprolactone diol/NDI prepolymer 90, catenary chain extender, and foaming chain extender composition 12.5.
The preparation process comprises the following steps: heating polycaprolactone diol to 100 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And mixing the dehydrated polycaprolactone diol with the molecular weight of 2000 and NDI-100 diisocyanate according to the ratio of 100:27 under the conditions of protection and medium-speed stirring, heating to 75 ℃, and stopping the reaction after the heat preservation is carried out for 3 hours to obtain the elastic main chain prepolymer, namely the polyurethane prepolymer.
In an inert gas N 2 Under the conditions of protection and stirring, mixing 500 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate according to a molar ratio of 1:1, heating to 50 ℃, and adding the total mass of the reaction raw material mixtureAnd (3) reacting for 2 hours with 5%o of T12 catalyst to stop the reaction, thereby obtaining the suspension chain extender.
The homogenizing emulsifier is prepared by mixing alkylphenol ethoxylate OP-10, sorbitan monooleate-80 and polysorbate-80 according to a ratio of 3:1:1.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, the 1, 4-butanediol, the catalyst and the homogenizing emulsifier are subjected to vacuum degassing until no bubble exists, and then are uniformly mixed with foaming agent water, and are emulsified on an emulsifying machine for 1 hour under high power for standby, wherein the suspension chain extender and the 1, 4-butanediol are prepared by the following steps: catalyst: the ratio of the homogenizing emulsifying agent to the water is 20:7:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 65 ℃ according to the formula proportion, rapidly stirring, heating to 90 ℃, preserving heat for 0.5h, curing, continuously heating to 120 ℃, preserving heat for 16h, and curing to obtain the polyurethane elastomer damping material.
The damping performance of the damping material obtained in the embodiment is characterized by a unimodal structure, the corresponding temperatures of damping peaks are-30 ℃, and the size distribution of cells is 80-180 mu m.
Comparative example 2 a polyurethane microporous elastomer double-peak damping material comprises the following components in parts by weight: polycaprolactone diol/TDI-100 prepolymer 100, catenary chain extender, and foaming chain extender composition 13.8.
The preparation process comprises the following steps: heating polycaprolactone diol to 110 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol; in an inert gas N 2 And under the protection and medium-speed stirring, mixing dehydrated polycaprolactone diol with 2000 molecular weight and TDI100 diisocyanate according to a ratio of 100:27, heating to 75 ℃, and stopping the reaction after heat preservation for 1h to obtain an elastic main chain prepolymer, namely a polyurethane prepolymer.
Under the protection of inert gas and stirring, mixing 2000 molecular weight polyethylene glycol monomethyl ether and isophorone diisocyanate according to a molar ratio of 1:1, heating to 50 ℃, adding 4%o of T12 catalyst (based on the total mass of the reaction raw material mixture), and stopping the reaction for 2 hours to obtain the suspension chain extender.
The catalyst was prepared from dibutyltin dilaurate and triethylenediamine in a weight ratio of 1:2.
The suspension chain extender, 1, 4-butanediol, a catalyst and a homogenizing emulsifier (alkylphenol ethoxylate OP-10) are subjected to vacuum degassing until no bubbles exist, then are uniformly mixed with foaming agent water, and are emulsified on an emulsifying machine for 1 hour under high power for standby, wherein the suspension chain extender, propylene glycol and 1, 4-butanediol are used: catalyst: the ratio of the foam homogenizing emulsifying agent to the water is 20:3.75:3.75:0.3:7.5:5.
In an inert gas N 2 Under the conditions of protection and stirring, adding a chain extender and a foaming chain extension composition into the polyurethane prepolymer at 72 ℃ according to the formula proportion, rapidly stirring, heating to 95 ℃, preserving heat for 0.5h, curing, continuously heating to 120 ℃, preserving heat for 18h, and curing to obtain the polyurethane elastomer damping material.
The damping material obtained in the embodiment has a damping performance characteristic of a double-peak structure, the corresponding temperatures of damping peaks are-27 ℃ and 34 ℃, and the size distribution of cells is 80-260 mu m.
The key to introducing side chains based on molecular design to create two damping peaks is that the molecular weight of the side chains, when below the critical value, is insufficient to create sufficient relaxation hysteresis, so that comparative example 1 does not exhibit bimodal character. When the molecular weight is large to a certain value, hysteresis is generated due to energy consumption such as entanglement with a main chain, hydrogen bond dissociation recombination and internal friction in the movement process, and a second damping peak is generated.
Cell size uniformity can be controlled with a verified combination of surfactants, and comparative example 2, which does not use this combination, has a larger cell size and a wider size distribution than the examples. The ratio provided when surfactants having different hydrophilic and lipophilic characteristics are used allows for both dispersion of water and polyol and control of the cell size distribution width.
The damping materials prepared in examples 1-6 and comparative examples 1-2, as well as existing BASF brand samples available on the market, were subjected to performance testing as follows:
Figure BDA0004083132120000081
as can be seen by comparing the performance of the comparative sample, the physical and mechanical properties of the formulation of the example are higher than those of the comparative sample in tensile strength and breaking productivity; the pressure resistance and the variable performance are superior to those of the comparative example and foreign products, the damping is of an obvious double-peak structure, and the high and low temperature is matched with the using temperature range of the household appliance, so that the damping has a good application prospect.

Claims (10)

1. A polyurethane microcellular elastomer damping material, characterized in that: the bimodal damping temperature is between minus 30 ℃ and minus 25 ℃ and between 30 ℃ and 40 ℃ respectively, and the foaming pore size distribution is between 50 and 180 mu m; the components of the composition are as follows in parts by weight: 70-100 parts of polyurethane prepolymer, 5-50 parts of suspension chain extender and foaming chain extender composition;
the suspension chain extender and the foaming chain extender composition thereof are a combination of the suspension chain extender, small molecular dihydric alcohol, a catalyst, a foam homogenizing emulsifier and a foaming agent, wherein the foaming agent is water;
the chain extender is obtained by reacting polyethylene glycol monomethyl ether and diisocyanate under the action of an organotin catalyst, wherein the molecular weight of the polyethylene glycol monomethyl ether is 1000-2000.
2. The polyurethane microcellular elastomer damping material according to claim 1, wherein: suspension chain extender: small molecule diols: catalyst: homogenizing emulsifying agent: the foaming agent is 18-22:3-6:0.2-0.4:6-9:4-6.
3. The polyurethane microcellular elastomer damping material according to claim 1, wherein: the foam homogenizing emulsifier is a mixture of alkylphenol ethoxylates OP-10, sorbitan monooleate-80 and polysorbate-80 in a weight ratio of 3:1:1.
4. The polyurethane microcellular elastomer damping material according to claim 1, wherein: the catalyst is an organotin and triethylenediamine combined catalyst, and the weight ratio of the organotin to triethylenediamine combined catalyst is preferably 1:2; the organotin is preferably dibutyltin dilaurate.
5. The polyurethane microcellular elastomer damping material according to claim 1, wherein: the micromolecular dihydric alcohol is one or two of ethylene glycol, propylene glycol, diethylene glycol and 1, 4-butanediol, and when the two are mixed for use, the mixing ratio is 1:1.
6. The polyurethane microcellular elastomer damping material according to claim 1, wherein: the diisocyanate in the suspension chain extender is isophorone diisocyanate.
7. The polyurethane microcellular elastomer damping material according to claim 1, wherein: the polyurethane prepolymer is obtained by reacting polyester diol with diisocyanate, wherein the weight ratio of the polyester diol to the diisocyanate is (70-100): (20-40); the polyester diol is one or more of polycaprolactone polyol, polyethylene glycol adipate and polybutylene adipate; the molecular weight of the polyester dihydric alcohol is 1000-2000; the diisocyanate is selected from TDI-100 and NDI.
8. The polyurethane microcellular elastomer damping material according to claim 1, wherein: the organotin catalyst is selected from dibutyltin dilaurate T12 or stannous octoate T9; the dosage of the organotin catalyst is 1 to 5 per mill of the total mass of the polyethylene glycol monomethyl ether and the diisocyanate; the mol ratio of polyethylene glycol monomethyl ether to diisocyanate is 1:1.
9. The method for preparing the polyurethane microporous elastomer damping material according to claim 1, which is characterized by comprising the following specific steps:
(1) Preparation of polyurethane prepolymers
Heating the polyester diol to 100-120 ℃, and carrying out vacuum dehydration to obtain dehydrated polyester diol;under the protection of inert gas and medium-speed stirring, mixing dehydrated polyester diol and diisocyanate, heating to 70-80 ℃, and stopping the reaction after heat preservation for 1-3 hours to obtain an elastic main chain prepolymer, namely polyurethane prepolymer; the inert gas is N 2 ；
(2) Suspension chain extender and preparation of foaming chain extender composition thereof
Vacuum degassing the suspension chain extender, the micromolecular dihydric alcohol, the catalyst and the homogenizing emulsifier until no bubbles exist, uniformly mixing the suspension chain extender, the micromolecular dihydric alcohol, the catalyst and the homogenizing emulsifier with the foaming agent, and emulsifying the mixture on an emulsifying machine for 1 hour under high power for standby;
(3) Preparation of polyurethane microporous elastomer damping material
In an inert gas N 2 Under the conditions of protection and stirring, adding the suspension chain extender and the foaming chain extender composition thereof into the polyurethane prepolymer at 65-90 ℃ according to a proportion, rapidly stirring, heating to 90-95 ℃, preserving heat for 0.5-2h, curing, continuously heating to 100-150 ℃, preserving heat for 10-26 h, and curing to obtain the polyurethane elastomer damping material.
10. The method for preparing a polyurethane microporous elastomer damping material according to claim 9, wherein:
the suspension chain extender is specifically prepared from the following steps: under the condition of inert gas protection and medium-speed stirring, mixing polyethylene glycol monomethyl ether and diisocyanate in equal quantity according to a molar ratio, heating to 50 ℃, adding an organotin catalyst, and stopping the reaction after 2 hours of reaction to obtain a suspension chain extender; the inert gas is N 2 。
CN202310128968.1A 2022-12-30 2023-02-17 Full-water foaming polyurethane microporous elastomer double-peak damping material based on molecular design and preparation method thereof Pending CN116333260A (en)

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