CN105732935A - Manufacturing method of polyurethane microporous elastomer - Google Patents
Manufacturing method of polyurethane microporous elastomer Download PDFInfo
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- CN105732935A CN105732935A CN201410756313.XA CN201410756313A CN105732935A CN 105732935 A CN105732935 A CN 105732935A CN 201410756313 A CN201410756313 A CN 201410756313A CN 105732935 A CN105732935 A CN 105732935A
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Abstract
The invention discloses a manufacturing method of polyurethane microporous elastomer. The method comprises technical processes including preparation of a pre-polymer, preparation of a chain extender, casting, and post-curing. According to the method, interior heat of a product is reduced, dynamic fatigue performance is improved, and service life of the product is prolonged. Application field of the elastomer can be further developed, and the elastomer can be mainly used to damping systems of automobiles, bridges, and elevators.
Description
Technical field
The preparation method that the present invention relates to a kind of microporous polyurethane elastomer, is mainly used in the shock absorption system of automobile bridge and elevator.
Background technology
Microporous polyurethane elastomer, also known as foaming polyurethanes elastomer, there is the excellent properties such as good mechanical property, abrasion performance, oil resistant, tear-resistant, resistance to chemical attack, resistance to x radiation x, cementability be good, especially MDI type polyurethane micro-pore elastomer, its vapour pressure, hypotoxicity is little, therefore for many years, people are being devoted to the exploitation of MDI type polyurethane always, and market share constantly rises.
Owing to microporous polyurethane elastomer polar groups is more, intramolecular force and intermolecular active force are bigger, add other factor hindering singly-bound to rotate freely that may be present, the ess-strain making microporous polyurethane elastomer can not reach balance moment, hysteresis is shown as under alternate stress effect, cause Nei Shengre, make material internal temperature suddenly raise, have a strong impact on the serviceability of goods.
nullThe preparation method that Chinese patent CN102304214B disclosed a kind of automobile microvoid polyurethane damping, buffering block on 03 13rd, 2013，Utilize the polyester lactone polyols that molecular weight is 6000-10000 as raw material，And introducing 2 ± 0.5Wt.% nano calcium carbonate micro powder improves dynamic endurance and the comprehensive mechanical property of product in polyether polyol，Preparation process needs add acetone equal solvent，Acetone toxicity is big compared with ethanol，And the molecular weight of polyester lactone is bigger，In use viscosity is bigger，Energy consumption is relatively many，The present invention is the polyhydric alcohol having selected molecular weight to be 1000～3000，And auxiliary agent is ethanol，And it is that nano-calcium carbonate addition is 5～10%，It is possible not only to reduce production cost，And the Nei Shengre of material can be reduced，Improve service life under severe conditions，Optimize the dynamic fatigue property of material.
Summary of the invention
Above-mentioned deficiency for prior art, according to embodiments of the invention, wish the preparation method proposing a kind of microporous polyurethane elastomer, aim to solve the problem that and buffer stopper is mainly used for 4, Nei Shengre in 4-methyl diphenylene diisocyanate (MDI) type polyurethane micro-pore elastomer, reduce Nei Shengre, improve its dynamic fatigue resistance energy.According to embodiment, the preparation method of a kind of microporous polyurethane elastomer provided by the invention, its innovative point is in that, including following step:
(1) preparation of performed polymer: be 1:(1～2 by mass ratio) ethanol add in reactor with the nano-calcium carbonate that particle diameter is 10～100nm and add surface conditioning agent, the mass ratio of nano-calcium carbonate and surface conditioning agent is 100:(1.5～2), heating is to 40 DEG C, stirring is to dispersed, add polyhydric alcohol, the mass ratio of polyhydric alcohol and nano-calcium carbonate is 100:(5～10), stirring, evacuation, add excessive polyisocyanates, react 1.5～3 hours when 70～90 DEG C, form the performed polymer of end-NCO base content≤10%；
(2) preparation of chain extender: little molecule dihydroxylic alcohols, water, siloxane foams stabilizer and catalyst Homogeneous phase mixing are configured to chain extender；
(3) cast: by performed polymer and chain extender 100:(5～12 by weight) mix after, implantation temperature is in the mould of 60～95 DEG C, the demoulding after precuring；
(4) post curing: by post curing 13～16 hours at 100～110 DEG C of the goods after the demoulding, prepares microporous polyurethane elastomer.
According to an embodiment, the mixture that polyhydric alcohol is one or both compositions in polytetrahydrofuran polyol, polyether polyol, polycaprolactone polyol, polyester ether polylol, polycarbonate polyol in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, described in step (1).
According to an embodiment, in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, the number-average molecular weight of the polyhydric alcohol described in step (1) is 1000～3000, and degree of functionality is 2.
According to an embodiment, in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, step (1) described polyisocyanates is 4,4-methyl diphenylene diisocyanates.
According to an embodiment, in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, surface conditioning agent is single oxyalkyl titanate coupling agent or aluminate coupling agent.
According to an embodiment, in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, in step (1), after addition polyhydric alcohol, mixing speed is 150 turns/min, and mixing time is 15～30min.
According to an embodiment, in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, in chain extender, the molecular weight of little molecule dihydroxylic alcohols is 62-200, consumption is chain extender gross mass the 84～97% of little molecule dihydroxylic alcohols；The consumption of water is the 0.5～4% of chain extender gross mass, it is preferable that 1～4%；The consumption of siloxane foams stabilizer is the 0.5～2.0% of chain extender gross mass；Catalyst is triethylene diamine, double; two (dimethylaminoethyl) ether, stannous octoate or dibutyl tin laurate, or other amines or organometallic catalysts.In chain extender, siloxane foams stabilizer determines microcellular structure composition.
According to an embodiment, in the preparation method of the aforementioned microporous polyurethane elastomer of the present invention, little molecule dihydroxylic alcohols is one or both the mixture in ethylene glycol, 1,3-PD, diethylene glycol, BDO, 1,6-hexanediol and diglycol.
Relative to prior art, embodiment and test example subsequently will demonstrate that, the present invention uses the polyhydric alcohol of molecular weight 1000～3000, there is the low dispersion being more beneficial for nano-calcium carbonate of viscosity, nano-calcium carbonate is to have quantum size effect and skin effect, the nano-calcium carbonate surface that surface treated is crossed is active, the microphase-separated of polyurethane is favourable, make polyurethane material fricative heat minimizing between soft segment in dynamic fatigue, reduce further the Nei Shengre of material and then the service life of the microporous polyurethane elastomer extended.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.These embodiments are interpreted as being merely to illustrate the present invention rather than limiting the scope of the invention.After having read the content that the present invention records, the present invention can be made various changes or modifications by those skilled in the art, and these equivalences change and modifications and fall into the scope of the claims in the present invention equally.
Embodiment 1
Adding reactor in nano-calcium carbonate according to the mass ratio of 1:1 by ethanol, the surface conditioning agent Aluminate of the 1.5% of addition nano-calcium carbonate quality and single oxyalkyl titanate coupling agent arrange according to the ratio of 1:2 and are mixed and heated to 40 DEG C, continue stirring 30min.The polycaprolactone diols of number-average molecular weight 2000 is joined in nano-calcium carbonate system, the amount accounting for polycaprolactone diols according to nano-calcium carbonate amount is 5% interpolation, stirring 20min, evacuation, intensification, 4 are added according to the amount of end-NCO%=8% after 3 hours, 4-methyl diphenylene diisocyanate, prepares performed polymer.
The preparation of chain extender, by BDO 100g, water 2g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.
The ratio that performed polymer and chain extender are components is 100:8.
Mixed by low-pressure blowing machine mixing performed polymer and chain extender component, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
Embodiment 2
The content of the nano-calcium carbonate in embodiment 1 is replaced with 8%, joins in the PolyTHF dihydroxylic alcohols that number-average molecular weight is 3000, stir 30min, evacuation, intensification, after 3 hours, add excessive 4,4-methyl diphenylene diisocyanate, prepares the performed polymer of-NCO%=7%.
Preparation chain extender component is: BDO 100g, water 1.5g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.
The ratio that performed polymer and chain extender are components is 100:7.
By low-pressure blowing machine by performed polymer and chain extender component mix homogeneously, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
Embodiment 3
Adding reactor in nano-calcium carbonate according to the mass ratio of 1:2 by ethanol, single oxyalkyl titanate esters of the 2% of addition nano-calcium carbonate quality heats to 40 DEG C, continues stirring 30min.The polyether Glycols of number-average molecular weight 2000 is joined in nano-calcium carbonate system, the amount accounting for polyether Glycols according to nano-calcium carbonate amount is 6% interpolation, stirring 20min, evacuation, intensification, 4 are added according to the amount of end-NCO%=10% after 3 hours, 4-methyl diphenylene diisocyanate, prepares performed polymer.
The preparation of chain extender, by BDO 95g, diglycol 5g, water 3g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.
The ratio that performed polymer and chain extender are components is 100:10.
By low-pressure blowing machine by performed polymer and chain extender component mix homogeneously, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
Embodiment 4
Adding reactor in nano-calcium carbonate according to the mass ratio of 1:1.8 by ethanol, single oxyalkyl titanate coupling agent of the 2% of addition nano-calcium carbonate quality heats to 40 DEG C, continues stirring 30min.The polyether ester dihydroxylic alcohols of number-average molecular weight 2000 is joined in nano-calcium carbonate system, the amount accounting for polyether ester dihydroxylic alcohols according to nano-calcium carbonate amount is 5% interpolation, stirring 15min, evacuation, intensification, 4 are added according to the amount of end-NCO%=8% after 3 hours, 4-methyl diphenylene diisocyanate, prepares performed polymer.
Preparation chain extender component BDO 100g, water 2.5g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.The ratio that performed polymer and chain extender are components is 100:8.
By low-pressure blowing machine by performed polymer and chain extender component mix homogeneously, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
Embodiment 5
Adding reactor in nano-calcium carbonate according to the mass ratio of 1:1.5 by ethanol, the aluminate coupling agent of the 1.5% of addition nano-calcium carbonate quality heats to 40 DEG C, continues stirring 30min.The polyether ester dihydroxylic alcohols of number-average molecular weight 2000 is joined in nano-calcium carbonate system, the amount accounting for polyether ester dihydroxylic alcohols according to nano-calcium carbonate amount is 9% interpolation, stirring 15min, evacuation, intensification, 4 are added according to the amount of end-NCO%=5% after 3 hours, 4-methyl diphenylene diisocyanate, prepares performed polymer.
Preparation chain extender component BDO 90g, 1,3-PD 10g, water 1g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.The ratio that performed polymer and chain extender are components is 100:5.
By low-pressure blowing machine by performed polymer and chain extender component mix homogeneously, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
Embodiment 6
Adding reactor in nano-calcium carbonate according to the mass ratio of 1:1.5 by ethanol, single oxyalkyl titanate coupling agent of the 1.5% of addition nano-calcium carbonate quality heats to 40 DEG C, continues stirring 30min.The PolyTHF dihydroxylic alcohols of number-average molecular weight 2000 is joined in nano-calcium carbonate system, the amount accounting for PolyTHF dihydroxylic alcohols according to nano-calcium carbonate amount is 7% interpolation, stirring 25min, evacuation, intensification, 4 are added according to the amount of end-NCO%=9% after 3 hours, 4-methyl diphenylene diisocyanate, prepares performed polymer.
Preparation chain extender component BDO 100g, water 4g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.The ratio that performed polymer and chain extender are components is 100:8.5.
By low-pressure blowing machine by performed polymer and chain extender component mix homogeneously, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
Comparative example 1
By the PolyTHF dihydroxylic alcohols that number-average molecular weight is 2000, evacuation, after 2 hours, adds 4,4-excessive methyl diphenylene diisocyanates, prepares the performed polymer of-NCO%=7%.
Preparation chain extender component BDO 100g, water 2g, foam stabiliser 2g, catalyst 0.3g mix homogeneously.The ratio that performed polymer and chain extender are components is 100:6.
By low-pressure blowing machine mixing performed polymer and chain extender component mix homogeneously, be poured into the in-mold molding of temperature 90 DEG C, after the demoulding in the baking oven of 110 DEG C post curing 15 hours.Then carry out post curing treatment, test the temperature rise in dynamic fatigue and other performances.
The performance test of above-described embodiment 1-6 and comparative example 1 is as shown in table 1.
As shown in table 1, frequency at 1.5HZ, the power of 6KN, when calm, embodiment 1-6 has minimizing in various degree at test body internal temperature after 200min, embodiment 2 dynamic fatigue rear profile internal temperature relatively comparative example 1 reduces 5 DEG C, hence it is evident that reduce the Nei Shengre of material, the service life of the material of raising.
As shown in table 1, through along the goods short transverse frequency with 2HZ, the 50% of compressed product height, altogether after 100,000 tests of circulation, height after survey goods fatigue, embodiment 1-6 relatively comparative example 1 increases to some extent, and wherein the dynamic fatigue deformation quantity of embodiment 3 relatively comparative example 1 decreases 38.9%, and maintain the strength of materials, and then while reducing material Nei Shengre, add the comprehensive mechanical property of material.
Table 1
Claims (9)
1. a preparation method for microporous polyurethane elastomer, is characterized in that, including following step:
(1) preparation of performed polymer: be 1:(1～2 by mass ratio) ethanol add in reactor with the nano-calcium carbonate that particle diameter is 10～100nm and add surface conditioning agent, the mass ratio of nano-calcium carbonate and surface conditioning agent is 100:(1.5～2), heating is to 40 DEG C, stirring is to dispersed, add polyhydric alcohol, the mass ratio of polyhydric alcohol and nano-calcium carbonate is 100:(5～10), stirring, evacuation, add excessive polyisocyanates, react 1.5～3 hours when 70～90 DEG C, form the performed polymer of end-NCO base content≤10%；
(2) preparation of chain extender: little molecule dihydroxylic alcohols, water, siloxane foams stabilizer and catalyst Homogeneous phase mixing are configured to chain extender；
(3) cast: by performed polymer and chain extender 100:(5～12 by weight) mix after, implantation temperature is in the mould of 60～95 DEG C, the demoulding after precuring；
(4) post curing: by post curing 13～16 hours at 100～110 DEG C of the goods after the demoulding, prepares microporous polyurethane elastomer.
2. the preparation method of microporous polyurethane elastomer according to claim 1, it is characterized in that, the mixture that polyhydric alcohol is one or both compositions in polytetrahydrofuran polyol, polyether polyol, polycaprolactone polyol, polyester ether polylol, polycarbonate polyol described in step (1).
3. the preparation method of microporous polyurethane elastomer according to claim 1, is characterized in that, the number-average molecular weight of the polyhydric alcohol described in step (1) is 1000～3000, and degree of functionality is 2.
4. the preparation method of microporous polyurethane elastomer according to claim 1, is characterized in that, step (1) described polyisocyanates is 4,4-methyl diphenylene diisocyanates.
5. the preparation method of microporous polyurethane elastomer according to claim 1, is characterized in that, surface conditioning agent is single oxyalkyl titanate coupling agent or aluminate coupling agent.
6. the preparation method of microporous polyurethane elastomer according to claim 1, is characterized in that, in step (1), after addition polyhydric alcohol, mixing speed is 150 turns/min, and mixing time is 15～30min.
7. the preparation method of microporous polyurethane elastomer according to claim 1, is characterized in that, in chain extender, the molecular weight of little molecule dihydroxylic alcohols is 62-200, consumption is chain extender gross mass the 84～97% of little molecule dihydroxylic alcohols；The consumption of water is the 0.5～4% of chain extender gross mass；The consumption of siloxane foams stabilizer is the 0.5～2.0% of chain extender gross mass；Catalyst is triethylene diamine, double; two (dimethylaminoethyl) ether, stannous octoate or dibutyl tin laurate.
8. the preparation method of microporous polyurethane elastomer according to claim 7, is characterized in that, little molecule dihydroxylic alcohols is one or both the mixture in ethylene glycol, 1,3-PD, diethylene glycol, BDO, 1,6-hexanediol and diglycol.
9. the preparation method of microporous polyurethane elastomer according to claim 7, is characterized in that, the consumption of water is the 1～4% of chain extender gross mass.
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| CN107868477A (en) * | 2017-10-31 | 2018-04-03 | 广州市白云化工实业有限公司 | Dual-component polyurethane modified liquid silicon rubber and preparation method thereof |
| CN109983048A (en) * | 2016-11-14 | 2019-07-05 | 巴斯夫欧洲公司 | The polyurethane elastomer of low resistance |
| CN117124525A (en) * | 2023-10-25 | 2023-11-28 | 河北铁科翼辰新材科技有限公司 | Preparation method of fatigue-resistant polyurethane microporous elastomer backing plate |
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| CN117124525A (en) * | 2023-10-25 | 2023-11-28 | 河北铁科翼辰新材科技有限公司 | Preparation method of fatigue-resistant polyurethane microporous elastomer backing plate |
| CN117124525B (en) * | 2023-10-25 | 2024-05-07 | 河北铁科翼辰新材科技有限公司 | Preparation method of fatigue-resistant polyurethane microporous elastomer backing plate |
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Effective date of registration: 20210623 Address after: 201201 area B, 1st floor, building 2, 813 Jianye Road, Pudong New Area, Shanghai Patentee after: SHANGHAI CARTHANE POLYURETHANE Co.,Ltd. Address before: 201201 No. 813 Jianye Road, Shanghai, Pudong New Area Patentee before: SHANGHAI CARTHANE Co.,Ltd. |