CN105732935B - A kind of preparation method of microporous polyurethane elastomer - Google Patents
A kind of preparation method of microporous polyurethane elastomer Download PDFInfo
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- CN105732935B CN105732935B CN201410756313.XA CN201410756313A CN105732935B CN 105732935 B CN105732935 B CN 105732935B CN 201410756313 A CN201410756313 A CN 201410756313A CN 105732935 B CN105732935 B CN 105732935B
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- polyurethane elastomer
- chain extender
- microporous polyurethane
- alcohol
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Abstract
The invention discloses the processing steps such as a kind of preparation method of microporous polyurethane elastomer, including the preparation of performed polymer, the preparation of chain extender, cast and post curing.The product prepared by the method for the invention can reduce the endogenous heat of material, improve dynamic fatigue property and increase service life, can further expand application field, be used primarily in the shock absorption system of automobile, bridge and elevator.
Description
Technical field
The present invention relates to a kind of preparation method of microporous polyurethane elastomer, it is mainly used for subtracting for automobile bridge and elevator
Shake system.
Background technology
Microporous polyurethane elastomer, also known as foaming polyurethanes elastomer have good mechanical property, abrasion performance, oil resistant, resistance to tear
It splits, is resistant to chemical etching, the excellent properties, especially MDI type polyurethanes micro-pore elastomer such as resistance to ray radiation, cementability are good, steaming
Vapour pressure, hypotoxicity is small, therefore for many years, and people are being dedicated to always the exploitation of MDI type polyurethanes, on occupation rate of market is continuous
It rises.
Since microporous polyurethane elastomer polar groups are more, intramolecular force and intermolecular active force are larger, then add
Upper other factors for interfering singly-bound to rotate freely that may be present so that the ess-strain of microporous polyurethane elastomer cannot moment
Reach balance, shows as hysteresis under alternate stress effect, cause endogenous heat, so that material internal temperature is increased suddenly, sternly
Ghost image rings the performance of product.
It is slow that Chinese patent CN102304214B disclosed a kind of automobile microvoid polyurethane damping on 03 13rd, 2013
The preparation method for rushing block, using the polyester lactone polyols that molecular weight is 6000-10000 as raw material, and in polyether polyol
Middle introducing 2 ± 0.5Wt.% nano calcium carbonate micro powders improve the dynamic endurance and comprehensive mechanical property of product, are preparing
It needs that acetone equal solvent is added in journey, acetone toxicity is big compared with ethyl alcohol, and the molecular weight of polyester lactone is larger, in use
Viscosity is larger, and energy consumption is relatively more, and the present invention is that have selected molecular weight be 1000~3000 polyalcohol, and auxiliary agent is second
Alcohol, and be nano-calcium carbonate additive amount 5~10%, production cost can be not only reduced, but also the interior of material can be reduced
Heat improves service life under severe conditions, optimizes the dynamic fatigue property of material.
Invention content
For the above-mentioned deficiency of the prior art, according to an embodiment of the invention, it is desirable to propose a kind of microporous polyurethane elasticity
The preparation method of body, it is intended to solve to be mainly used for 4,4- methyl diphenylene diisocyanates (MDI) type polyurethane in buffer stopper
Endogenous heat in micro-pore elastomer reduces endogenous heat, improves its dynamic fatigue resistance energy.It is provided by the invention according to embodiment
A kind of preparation method of microporous polyurethane elastomer, innovative point is, including following steps:
(1) preparation of performed polymer:It is 1 by mass ratio:The ethyl alcohol of (1~2) and the nano-calcium carbonate that grain size is 10~100nm
It is added in reaction kettle and is added surface conditioning agent, the mass ratio of nano-calcium carbonate and surface conditioning agent is 100:(1.5~2), add
Heat is stirred until homogeneous dispersion to 40 DEG C, adds polyalcohol, and the mass ratio of polyalcohol and nano-calcium carbonate is 100:(5~10),
Stirring, vacuumizes, excessive polyisocyanates is added, reacted 1.5~3 hours under conditions of 70~90 DEG C, forms end-NCO
The performed polymer of base content≤10%;
(2) preparation of chain extender:By small molecule dihydric alcohol, water, siloxane foams stabilizer and catalyst, uniformly mixing is matched
Chain extender is made;
(3) it pours into a mould:By performed polymer and chain extender by weight 100:(5~12) after mixing, implantation temperature is 60~95 DEG C
Mold in, demoulded after precuring;
(4) post curing:By the product after demoulding at 100~110 DEG C post curing 13~16 hours, be made microporous polyurethane
Elastomer.
It is more described in step (1) in the preparation method of aforementioned microporous polyurethane elastomer of the invention according to one embodiment
First alcohol is polytetrahydrofuran polyol, polyether polyol, polycaprolactone polyol, polyester ether polylol, polycarbonate polyol
One or both of composition mixture.
It is more described in step (1) in the preparation method of aforementioned microporous polyurethane elastomer of the invention according to one embodiment
The number-average molecular weight of first alcohol is 1000~3000, degree of functionality 2.
According to one embodiment, in the preparation method of aforementioned microporous polyurethane elastomer of the invention, step (1) described polyisocyanate
Cyanate is 4,4- methyl diphenylene diisocyanates.
According to one embodiment, in the preparation method of aforementioned microporous polyurethane elastomer of the invention, surface conditioning agent is single
Oxyalkyl titanate coupling agent or aluminate coupling agent.
According to one embodiment, in the preparation method of aforementioned microporous polyurethane elastomer of the invention, in step (1), it is added
Mixing speed is 150 turns/min after polyalcohol, and mixing time is 15~30min.
According to one embodiment, in the preparation method of aforementioned microporous polyurethane elastomer of the invention, in chain extender, small molecule
The molecular weight of dihydric alcohol is 62-200, and the dosage of small molecule dihydric alcohol is the 84~97% of chain extender gross mass;The dosage of water is
The 0.5~4% of chain extender gross mass, preferably 1~4%;The dosage of siloxane foams stabilizer be chain extender gross mass 0.5~
2.0%;Catalyst is triethylene diamine, bis- (dimethylaminoethyl) ethers, stannous octoate or dibutyl tin laurate, Huo Zheqi
His amine or organometallic catalysts.Siloxane foams stabilizer determines microcellular structure ingredient in chain extender.
According to one embodiment, in the preparation method of aforementioned microporous polyurethane elastomer of the invention, small molecule dihydric alcohol is
One or both of ethylene glycol, 1,3- propylene glycol, diethylene glycol, 1,4- butanediols, 1,6-HD and diglycol
Mixture.
Compared with the existing technology, subsequent embodiment and test example will demonstrate that, the present invention uses molecular weight 1000~3000
Polyalcohol, have the low dispersion for being more advantageous to nano-calcium carbonate of viscosity, nano-calcium carbonate is with quantum size effect and table
Face effect, the nano-calcium carbonate surface that surface treated is crossed is active, advantageous to the microphase-separated of polyurethane so that polyurethane
Material rub between soft segment in dynamic fatigue generation heat reduce, further reduced the endogenous heat of material, Jin Eryan
The service life of long microporous polyurethane elastomer.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.These embodiments are interpreted as being merely to illustrate this hair
It is bright rather than limit the scope of the invention.After having read the content of the invention recorded, those skilled in the art can
To be made various changes or modifications to the present invention, these equivalence changes and modification equally fall into model defined by the claims in the present invention
It encloses.
Embodiment 1
By ethyl alcohol and nano-calcium carbonate according to 1:1 mass ratio is added in reaction kettle, and nano-calcium carbonate quality is added
1.5% surface conditioning agent Aluminate is with single oxyalkyl titanate coupling agent according to 1:2 ratio row are mixed and heated to 40 DEG C, continue
Stir 30min.The polycaprolactone diols of number-average molecular weight 2000 is added in nano-calcium carbonate system, according to nano-calcium carbonate
The amount that calcium amount accounts for polycaprolactone diols is 5% addition, stirs 20min, vacuumizes, heats up, according to end-NCO%=after 3 hours
4,4- methyl diphenylene diisocyanates are added in 8% amount, and performed polymer is made.
1,4-butanediol 100g, water 2g, foam stabiliser 2g, catalyst 0.3g are uniformly mixed by the preparation of chain extender.
Performed polymer and chain extender are that the ratio of component is 100:8.
It is mixed by low-pressure blowing machine mixing performed polymer and chain extender component, is poured into the in-mold molding of 90 DEG C of temperature,
After demoulding in 110 DEG C of baking oven 15 hours of post curing.Then carry out post curing processing, test dynamic fatigue in temperature rise and
Other performances.
Embodiment 2
The content of nano-calcium carbonate in embodiment 1 is replaced with 8%, is added to the poly- tetrahydrochysene that number-average molecular weight is 3000
In furans dihydric alcohol, 30min is stirred, vacuumizes, heat up, after 3 hours, excessive 4,4- diphenylmethane diisocyanates are added
The performed polymer of-NCO%=7% is made in ester.
Preparing chain extender component is:1,4-butanediol 100g, water 1.5g, foam stabiliser 2g, catalyst 0.3g mixing are equal
It is even.
Performed polymer and chain extender are that the ratio of component is 100:7.
Performed polymer and chain extender component are uniformly mixed by low-pressure blowing machine, be poured into the mold of 90 DEG C of temperature at
Type, after demoulding in 110 DEG C of baking oven 15 hours of post curing.Then post curing processing is carried out, the temperature in dynamic fatigue is tested
Liter and other performances.
Embodiment 3
By ethyl alcohol and nano-calcium carbonate according to 1:2 mass ratio is added in reaction kettle, and the 2% of nano-calcium carbonate quality is added
Single oxyalkyl titanate esters be heated to 40 DEG C, continue stir 30min.The polyether Glycols of number-average molecular weight 2000 are added to and are received
In rice calcium carbonate system, the amount that polyether Glycols are accounted for according to nano-calcium carbonate amount is 6% addition, stirs 20min, vacuumizes, rises
4,4- methyl diphenylene diisocyanates are added according to the amount of end-NCO%=10% after 3 hours in temperature, and performed polymer is made.
The preparation of chain extender, by 1,4-butanediol 95g, diglycol 5g, water 3g, foam stabiliser 2g, catalyst
0.3g is uniformly mixed.
Performed polymer and chain extender are that the ratio of component is 100:10.
Performed polymer and chain extender component are uniformly mixed by low-pressure blowing machine, be poured into the mold of 90 DEG C of temperature at
Type, after demoulding in 110 DEG C of baking oven 15 hours of post curing.Then post curing processing is carried out, the temperature in dynamic fatigue is tested
Liter and other performances.
Embodiment 4
By ethyl alcohol and nano-calcium carbonate according to 1:1.8 mass ratio is added in reaction kettle, and nano-calcium carbonate quality is added
2% single oxyalkyl titanate coupling agent is heated to 40 DEG C, continues to stir 30min.By the polyether ester two of number-average molecular weight 2000
First alcohol is added in nano-calcium carbonate system, and the amount that polyether ester dihydric alcohol is accounted for according to nano-calcium carbonate amount is 5% addition, stirring
15min vacuumizes, heats up, and 4,4- methyl diphenylene diisocyanates, system is added according to the amount of end-NCO%=8% after 3 hours
Obtain performed polymer.
Chain extender component 1,4-butanediol 100g, water 2.5g, foam stabiliser 2g is prepared, catalyst 0.3g is uniformly mixed.
Performed polymer and chain extender are that the ratio of component is 100:8.
Performed polymer and chain extender component are uniformly mixed by low-pressure blowing machine, be poured into the mold of 90 DEG C of temperature at
Type, after demoulding in 110 DEG C of baking oven 15 hours of post curing.Then post curing processing is carried out, the temperature in dynamic fatigue is tested
Liter and other performances.
Embodiment 5
By ethyl alcohol and nano-calcium carbonate according to 1:1.5 mass ratio is added in reaction kettle, and nano-calcium carbonate quality is added
1.5% aluminate coupling agent is heated to 40 DEG C, continues to stir 30min.The polyether ester dihydric alcohol of number-average molecular weight 2000 is added
Enter into nano-calcium carbonate system, the amount that polyether ester dihydric alcohol is accounted for according to nano-calcium carbonate amount is 9% addition, stirs 15min, is taken out
4,4- methyl diphenylene diisocyanates are added according to the amount of end-NCO%=5% after 3 hours in vacuum, heating, and pre-polymerization is made
Body.
Prepare chain extender component 1,4-butanediol 90g, 1,3-PD 10g, water 1g, foam stabiliser 2g, catalyst
0.3g is uniformly mixed.Performed polymer and chain extender are that the ratio of component is 100:5.
Performed polymer and chain extender component are uniformly mixed by low-pressure blowing machine, be poured into the mold of 90 DEG C of temperature at
Type, after demoulding in 110 DEG C of baking oven 15 hours of post curing.Then post curing processing is carried out, the temperature in dynamic fatigue is tested
Liter and other performances.
Embodiment 6
By ethyl alcohol and nano-calcium carbonate according to 1:1.5 mass ratio is added in reaction kettle, and nano-calcium carbonate quality is added
1.5% single oxyalkyl titanate coupling agent is heated to 40 DEG C, continues to stir 30min.By the poly- tetrahydrochysene of number-average molecular weight 2000
Furans dihydric alcohol is added in nano-calcium carbonate system, and the amount that PolyTHF dihydric alcohol is accounted for according to nano-calcium carbonate amount is 7%
Addition stirs 25min, vacuumizes, heats up, different according to the amount of end-NCO%=9% addition 4,4- diphenyl methanes two after 3 hours
Performed polymer is made in cyanate.
Chain extender component 1,4-butanediol 100g, water 4g, foam stabiliser 2g is prepared, catalyst 0.3g is uniformly mixed.In advance
Aggressiveness and chain extender are that the ratio of component is 100:8.5.
Performed polymer and chain extender component are uniformly mixed by low-pressure blowing machine, be poured into the mold of 90 DEG C of temperature at
Type, after demoulding in 110 DEG C of baking oven 15 hours of post curing.Then post curing processing is carried out, the temperature in dynamic fatigue is tested
Liter and other performances.
Comparative example 1
After vacuumizing 2 hours, excessive 4,4- hexichol is added in the PolyTHF dihydric alcohol for being 2000 by number-average molecular weight
The performed polymer of-NCO%=7% is made in dicyclohexylmethane diisocyanate.
Chain extender component 1,4-butanediol 100g, water 2g, foam stabiliser 2g is prepared, catalyst 0.3g is uniformly mixed.In advance
Aggressiveness and chain extender are that the ratio of component is 100:6.
Be uniformly mixed by low-pressure blowing machine mixing performed polymer and chain extender component, be poured into the mold of 90 DEG C of temperature at
Type, after demoulding in 110 DEG C of baking oven 15 hours of post curing.Then post curing processing is carried out, the temperature in dynamic fatigue is tested
Liter 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, in the frequency of 1.5HZ, the power of 6KN, under conditions of calm, embodiment 1-6 is after 200min
Test body internal temperature has different degrees of reduction, and 2 dynamic fatigue rear profile internal temperature of embodiment is compared with comparative example 1
Reduce 5 DEG C, hence it is evident that reduce the endogenous heat of material, the service life of the material of raising.
As shown in table 1, by along product short transverse with the frequency of 2HZ, the 50% of compressed product height, recycle 10 altogether
After ten thousand tests, height after product fatigue is surveyed, embodiment 1-6 increased compared with comparative example 1, and wherein embodiment 3 is more right
Dynamic fatigue deformation quantity than embodiment 1 reduces 38.9%, and maintains the strength of materials, and then is reducing material endogenous heat
While increase the comprehensive mechanical property of material.
Table 1
Claims (10)
1. a kind of preparation method of microporous polyurethane elastomer, characterized in that including following steps:
(1) preparation of performed polymer:It is 1 by mass ratio:The ethyl alcohol of (1~2) is added with the nano-calcium carbonate that grain size is 10~100nm
In reaction kettle and it is added surface conditioning agent, the mass ratio of nano-calcium carbonate and surface conditioning agent is 100:(1.5~2), are heated to
40 DEG C, it is stirred until homogeneous dispersion, adds polyalcohol, the mass ratio of polyalcohol and nano-calcium carbonate is 100:(5~10), are stirred
It mixes, vacuumizes, excessive polyisocyanates is added, reacted 1.5~3 hours under conditions of 70~90 DEG C, form end-NCO bases
The performed polymer of content≤10%;The number-average molecular weight of the polyalcohol is 1000~2000;
(2) preparation of chain extender:Small molecule dihydric alcohol, water, siloxane foams stabilizer and catalyst are uniformly hybridly prepared into
Chain extender;
(3) it pours into a mould:By performed polymer and chain extender by weight 100:(5~12) after mixing, implantation temperature is 60~95 DEG C of mould
In tool, demoulded after precuring;
(4) post curing:By the product after demoulding, post curing 13~16 hours, obtained microporous polyurethane are elastic at 100~110 DEG C
Body.
2. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that more described in step (1)
First alcohol is one or both of polyether polyol, polycaprolactone polyol, polyester ether polylol, polycarbonate polyol composition
Mixture.
3. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that more described in step (1)
The degree of functionality of first alcohol is 2.
4. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that step (1) described polyisocyanate
Cyanate is 4,4- methyl diphenylene diisocyanates.
5. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that surface conditioning agent is single oxygen
Alkyl titanate coupling agent or aluminate coupling agent.
6. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that in step (1), be added more
Mixing speed is 150 turns/min after first alcohol, and mixing time is 15~30min.
7. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that in chain extender, small molecule
The molecular weight of dihydric alcohol is 62-200, and the dosage of small molecule dihydric alcohol is the 84~97% of chain extender gross mass;The dosage of water is
The 0.5~4% of chain extender gross mass;The dosage of siloxane foams stabilizer is the 0.5~2.0% of chain extender gross mass;Catalysis
Agent is triethylene diamine, bis- (dimethylaminoethyl) ethers, stannous octoate or dibutyl tin laurate.
8. the preparation method of microporous polyurethane elastomer according to claim 7, characterized in that small molecule dihydric alcohol is second
One or both of glycol, 1,3- propylene glycol, diethylene glycol, 1,4- butanediols, 1,6-HD and diglycol
Mixture.
9. the preparation method of microporous polyurethane elastomer according to claim 7, characterized in that the dosage of water is chain extender
The 1~4% of gross mass.
10. the preparation method of microporous polyurethane elastomer according to claim 1, characterized in that more described in step (1)
First alcohol is polytetrahydrofuran polyol.
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CN106317857B (en) * | 2016-08-18 | 2019-09-17 | 中国工程物理研究院化工材料研究所 | The polyurethane elastomeric compositions and preparation method thereof of urea groups paraffin swarms body |
EP3538580A1 (en) * | 2016-11-14 | 2019-09-18 | Basf Se | Low-damping polyurethane elastomer |
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 |
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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CN101838458A (en) * | 2010-04-07 | 2010-09-22 | 张家港市源丰科技发展有限公司 | Method for manufacturing polyurethane microporous automotive buffer block |
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WO2009009571A1 (en) * | 2007-07-12 | 2009-01-15 | Dow Global Technologies Inc. | Prepolymers and polymers for elastomers |
CN101838458A (en) * | 2010-04-07 | 2010-09-22 | 张家港市源丰科技发展有限公司 | Method for manufacturing polyurethane microporous automotive buffer block |
CN102304214A (en) * | 2011-07-19 | 2012-01-04 | 奥斯汀新材料(张家港)有限公司 | Method for preparing micropore polyurethane vibration reduction buffering block for automobile |
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