CN1803919A - Method for preparing nano silicon dioxide reinforced polyurethane road crack filling material - Google Patents
Method for preparing nano silicon dioxide reinforced polyurethane road crack filling material Download PDFInfo
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- CN1803919A CN1803919A CN 200610049190 CN200610049190A CN1803919A CN 1803919 A CN1803919 A CN 1803919A CN 200610049190 CN200610049190 CN 200610049190 CN 200610049190 A CN200610049190 A CN 200610049190A CN 1803919 A CN1803919 A CN 1803919A
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Abstract
The provided polyurethane reinforced by nano-SiO2 as road joint sealing material is prepared by mixing A and B constituents; wherein, A comprises the polyurethane prepolymer composed by bifunctional and trifunctional polyether alcohols with molecular weight as 1000-3000 and TDI, and B contains the acetone solution with 3, 3'- dichloro-4, 4'-diaminodiphenylmethane (MOCA) and other auxiliary agent. This product has well tensile property, adjustable gelling time and super cohesive force with cement-concrete road surface, and can replace the traditional bitumen or the modified to meet the request from high-level highway and airfield runway.
Description
Technical field
The present invention relates to a kind of preparation method of nano silicon enhanced polyurethane road crack filling material.
Background technology
The relatively poor asphalt mixture of use properties mostly in the pavement joint sealing material uses the burnt mud of polyvinyl chloride etc. on a small quantity.Traditional pitch or modifying asphalt seam sealer have the following shortcoming: (1) seam sealer and cement concrete concrete plate cohesive force are poor, and easy and cement concrete is thrown off; (2) seam sealer heatproof degree poor stability causes easy fusion in summer to extrude the road surface, easy embrittlement in winter cracking, and life cycle is shorter, need often overhaul, thereby cause the waste of lot of manpower and material resources.
Polyurethane material itself has good high and low temperature resistance, mechanical property preferably, and have certain cohesiveness with other material.But with its pointing as anti-impact and resistance to compression road surface, above-mentioned performance is still waiting to improve.Other performance such as high workability and ambient cure also must possess.Oneself has a large amount of reports to inorganic nano material as additive improved macromolecular material performance, has gratifying application prospect.Adopt inorganic nano-particle (SiO in this patent
2) the in-situ hybridization polymerization prepares urethane, make and contain inorganic nano-particle SiO
2The polyurethane hybrid thing forms cross-linked network structure, improved material tensile strength and with inorganic cement concrete adhesive property; Owing in preparation, also adopted the B component that contains compositions such as chainextender-organic solvent, make this pointing not only have ambient cure but also have good mobility again.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nano silicon enhanced polyurethane road crack filling material.
The step of method is as follows:
1) will measure 10-20 part 3,3 '-two chloro-4 under 20-30 ℃, 4 '-diamines ditan is dissolved in the acetone of 20-30 part, adds dibutyl phthalate and obtains chainextender.
2) with 100 parts of polyethers 210, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, 1-10 part nanometer silicon dioxide particle is joined polyethers 210 back high speed dispersion 2-3 hour of above-mentioned dehydration, add product that the reaction of 20-40 part tolylene diisocyanate produces with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by the mixed of 80-100: 10-60;
3) 10-30 part chainextender is added 80-100 part base polyurethane prepolymer for use as component, under 20-30 ℃, mix and obtained light yellow transparent joint filling slurry in 5-15 minute and get final product.
Described nano silicon particle diameter is 30-50nm, and two functionality Aethoxy Sklerol molecular weight are 1000-3000g/mol, and three-functionality-degree Aethoxy Sklerol molecular weight is 1000-3000g/mol.
Advantage of the present invention is to be toughener with the nano silicon, has prepared a kind of urethane gap-grouting material of inorganic-organic hybridization.Introduce specific inorganic nano-particle (SiO
2) make the polyurethane hybrid structure form cross-linked network, improved the tensile property of material, and superior bond strengths rendering has been arranged.
Embodiment
Following examples provides the preparation method that nano silicon strengthens polyurethane filling material.Yet these embodiment only provide explanation rather than restriction the present invention.
Below be the umber of implementing, all by weight.
Embodiment 1
1) will measure down in the acetone that 15 parts of MOCA are dissolved in 23 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 1 part of nanometer silicon dioxide particle joined above-mentioned dehydration are standby after 2-3 hour.Add 30 parts of tolylene diisocyanates in the reactor, be warming up to 60-70 ℃, the mixture of the above-mentioned polyethers-nano silicon that has prepared is slowly dropped in the reactor, reaction is 2-3 hour about 75-85 ℃, and discharging barrelling sealing is standby.
3) 28 parts of chainextenders are added 100 parts of base polyurethane prepolymer for use as components, under 20-30 ℃, mix and obtained light yellow transparent joint filling slurry in 5-15 minute and get final product.Its key technical indexes is: slurries initial viscosity 15.7 pools under 30 ℃ probe temperature, and gel time 30min, its tensile strength 11.11MPa after the sample solidifies, elongation at break are 563.30% cohesive strength 6.5MPa.
Embodiment 2
1) will measure down in the acetone that 15 parts of MOCA are dissolved in 23 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 2 parts of nanometer silicon dioxide particles joined above-mentioned dehydration are standby after 2-3 hour.Add 30 parts of tolylene diisocyanates in the reactor, be warming up to 60-70 ℃, the mixture of the above-mentioned polyethers-nano silicon that has prepared is slowly dropped in the reactor, reaction is 2-3 hour about 75-85 ℃, and discharging barrelling sealing is standby.
3) 28 parts of chainextenders are added 100 parts of base polyurethane prepolymer for use as components, under 20-30 ℃, mix and obtained light yellow transparent joint filling slurry in 5-15 minute and get final product.Its key technical indexes is: slurries initial viscosity 16.7 pools under 30 ℃ probe temperature, and gel time 28min, its tensile strength 12.11MPa after the sample solidifies, elongation at break are 663.30% cohesive strength 7.5MPa.
Embodiment 3
1) will measure down in the acetone that 17 parts of MOCA are dissolved in 26 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 1 part of nanometer silicon dioxide particle joined above-mentioned dehydration are standby after 2-3 hour.In reactor, add 30 parts of tolylene diisocyanates, be warming up to 60-70 ℃, slowly drop to the mixture of the above-mentioned polyethers-nano silicon that has prepared in the reactor, about 75-85 ℃ the reaction 2-3 hour with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by 100: 10 mixed.
3) 100 parts of base polyurethane prepolymer for use as components and 32 parts of chainextenders are mixed under 25 ℃ can get light yellow transparent joint filling slurry in 10 minutes, its the key technical indexes is: slurries initial viscosity 16.74 pools under 30 ℃ probe temperature, gel time 27min, sample solidifies back draft intensity 13.80MPa, elongation at break are 537.72% cohesive strength 7.90MPa.
Embodiment 4
1) will measure down in the acetone that 18 parts of MOCA are dissolved in 27 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 1 part of nanometer silicon dioxide particle joined above-mentioned dehydration are standby after 2-3 hour.In reactor, add 30 parts of tolylene diisocyanates, be warming up to 60-70 ℃, slowly drop to the mixture of the above-mentioned polyethers-nano silicon that has prepared in the reactor, about 75-85 ℃ the reaction 2-3 hour with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by 100: 20 mixed.
3) 100 parts of base polyurethane prepolymer for use as components and 33 parts of chainextenders are mixed under 25 ℃ can get light yellow transparent joint filling slurry in 10 minutes, its the key technical indexes is: slurries initial viscosity 20.88 pools under 30 ℃ probe temperature, gel time 31min, sample solidifies back draft intensity is 10.87MPa, and elongation at break is 502.01% cohesive strength 6.34MPa.
Embodiment 5
1) will measure down in the acetone that 19 parts of MOCA are dissolved in 29 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 1 part of nanometer silicon dioxide particle joined above-mentioned dehydration are standby after 2-3 hour.In reactor, add 30 parts of tolylene diisocyanates, be warming up to 60-70 ℃, slowly drop to the mixture of the above-mentioned polyethers-nano silicon that has prepared in the reactor, about 75-85 ℃ the reaction 2-3 hour with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by 100: 40 mixed.
3) 100 parts of base polyurethane prepolymer for use as components and 36 parts of chainextenders are mixed under 25 ℃ can get light yellow transparent joint filling slurry in 10 minutes, its the key technical indexes is: slurries initial viscosity 15.4 pools under 30 ℃ probe temperature, gel time 27min, sample solidifies back draft intensity 13.66MPa, elongation at break are 392.57% cohesive strength 6.93Mpa.
Embodiment 6
1) will measure down in the acetone that 20 parts of MOCA are dissolved in 30 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 1 part of nanometer silicon dioxide particle joined above-mentioned dehydration are standby after 2-3 hour.In reactor, add 30 parts of tolylene diisocyanates, be warming up to 60-70 ℃, slowly drop to the mixture of the above-mentioned polyethers-nano silicon that has prepared in the reactor, about 75-85 ℃ the reaction 2-3 hour with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by 100: 50 mixed.
3) 100 parts of base polyurethane prepolymer for use as components and 38 parts of chainextenders are mixed under 25 ℃ can get light yellow transparent joint filling slurry in 10 minutes, its the key technical indexes is: slurries initial viscosity 14.4 pools under 30 ℃ probe temperature, gel time 28min, sample solidifies back draft intensity 12.66MPa, elongation at break are 405.57% cohesive strength 6.33Mpa.
Embodiment 7
1) will measure down in the acetone that 20 parts of MOCA are dissolved in 30 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) with 100 parts of polyethers 210 100-120 ℃ of following vacuum hydro-extraction 2 hours, the polyethers 210 back high speed dispersion that 1 part of nanometer silicon dioxide particle joined above-mentioned dehydration are standby after 2-3 hour.In reactor, add 30 parts of tolylene diisocyanates, be warming up to 60-70 ℃, slowly drop to the mixture of the above-mentioned polyethers-nano silicon that has prepared in the reactor, about 75-85 ℃ the reaction 2-3 hour with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by 100: 60 mixed.
3) 100 parts of base polyurethane prepolymer for use as components and 39 parts of chainextenders are mixed under 25 ℃ can get light yellow transparent joint filling slurry in 10 minutes, its the key technical indexes is: slurries initial viscosity 15.4 pools under 30 ℃ probe temperature, gel time 24min, sample solidifies back draft intensity 13.86MPa, elongation at break are 397.57% cohesive strength 7.33Mpa.
Embodiment 8
1) will measure down in the acetone that 28 parts of MOCA are dissolved in 42 parts at 25 ℃, obtain chainextender after adding a little dibutyl phthalate.
2) by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that adds 10-20 part tolylene diisocyanate reaction production was the base polyurethane prepolymer for use as component.
3) 100 parts of base polyurethane prepolymer for use as components and 70 parts of chainextenders are mixed under 25 ℃ can get light yellow transparent joint filling slurry in 10 minutes, its the key technical indexes is: slurries initial viscosity 17.4 pools under 30 ℃ probe temperature, gel time 29min, sample solidifies back draft intensity 14.66MPa, elongation at break are 398.57% cohesive strength 6.73Mpa.
Claims (4)
1. the preparation method of a nano silicon enhanced polyurethane road crack filling material is characterized in that, the step of method is as follows:
1) will measure 10-20 part 3,3 '-two chloro-4 under 20-30 ℃, 4 '-diamines ditan (MOCA) is dissolved in the acetone of 20-30 part, adds dibutyl phthalate and obtains chainextender.
2) with 100 parts of polyethers 210, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, 1-10 part nanometer silicon dioxide particle is joined polyethers 210 back high speed dispersion 2-3 hour of above-mentioned dehydration, add product that the reaction of 20-40 part tolylene diisocyanate produces with by 100 parts of polyethers 330, at 100-120 ℃ of following vacuum hydro-extraction 1-3 hour, the product that the reaction of adding 10-20 part tolylene diisocyanate is produced obtained the base polyurethane prepolymer for use as component by the mixed of 80-100: 10-60;
3) 10-30 part chainextender is added 80-100 part base polyurethane prepolymer for use as component, under 20-30 ℃, mix and obtained light yellow transparent joint filling slurry in 5-15 minute and get final product.
2. the preparation method of a kind of nano silicon enhanced polyurethane road crack filling material according to claim 1 is characterized in that, described nano silicon particle diameter is 30-50nm.
3. the preparation method of a kind of nano silicon enhanced polyurethane road crack filling material according to claim 1 is characterized in that, described two functionality Aethoxy Sklerol molecular weight are 1000-3000g/mol.
4. the preparation method of a kind of nano silicon enhanced polyurethane road crack filling material according to claim 1 is characterized in that, described three-functionality-degree Aethoxy Sklerol molecular weight is 1000-3000g/mol.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059555A (en) * | 2013-01-17 | 2013-04-24 | 浙江亿诚聚氨酯制造有限公司 | Nano-composite polyether thermoplastic polyurethane elastomer composition and preparation method thereof |
| CN106833383A (en) * | 2017-02-23 | 2017-06-13 | 山东科达基建有限公司 | A kind of road and bridge filleting method and filleting pitch are combined |
| CN107540275A (en) * | 2017-08-22 | 2018-01-05 | 安徽艾米伦特建材科技有限公司 | Insulation material and preparation method thereof |
| CN109553745A (en) * | 2018-10-22 | 2019-04-02 | 天津昌海新材料科技发展有限公司 | A kind of graphene modified high-weatherability height rebound nano-high molecule pointing and preparation method thereof |
| CN110293646A (en) * | 2019-06-10 | 2019-10-01 | 长兴正发热电耐火材料有限公司 | A kind of production technology of lightweight heat-proof joint sealing material |
| CN113462275A (en) * | 2021-06-30 | 2021-10-01 | 海星(深圳)高新技术研发有限公司 | Preparation method of nano coating liquid |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1501858A (en) * | 1974-07-12 | 1978-02-22 | Ici Ltd | Solid unfoamed urea copolymer compositions containing silica |
| CA1251294A (en) * | 1983-04-22 | 1989-03-14 | Mobay Chemical Corporation | Polyether polyurethane prepolymers and cast elastomers made therefrom |
| CN1140583C (en) * | 2000-11-15 | 2004-03-03 | 北京中商世纪纳米塑胶材料有限公司 | Spreading material for sports ground prepared from polyurethane/nanometer montorillonoid and its preparing method |
| CN1254494C (en) * | 2003-08-01 | 2006-05-03 | 北京新世纪纳米塑胶材料有限公司 | Stadium paving material prepared from nano polyurethane elastomer and its preparing method |
| CN1295288C (en) * | 2004-06-10 | 2007-01-17 | 北京宝利通纳米橡塑材料有限公司 | Sports ground paving material prepared with nanometer montmorillonite and polyurethane plastic and its prepn process |
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- 2006-01-20 CN CNB2006100491901A patent/CN100365066C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059555A (en) * | 2013-01-17 | 2013-04-24 | 浙江亿诚聚氨酯制造有限公司 | Nano-composite polyether thermoplastic polyurethane elastomer composition and preparation method thereof |
| CN103059555B (en) * | 2013-01-17 | 2014-12-03 | 浙江亿诚聚氨酯制造有限公司 | Nano-composite polyether thermoplastic polyurethane elastomer composition and preparation method thereof |
| CN106833383A (en) * | 2017-02-23 | 2017-06-13 | 山东科达基建有限公司 | A kind of road and bridge filleting method and filleting pitch are combined |
| CN107540275A (en) * | 2017-08-22 | 2018-01-05 | 安徽艾米伦特建材科技有限公司 | Insulation material and preparation method thereof |
| CN109553745A (en) * | 2018-10-22 | 2019-04-02 | 天津昌海新材料科技发展有限公司 | A kind of graphene modified high-weatherability height rebound nano-high molecule pointing and preparation method thereof |
| CN109553745B (en) * | 2018-10-22 | 2021-02-05 | 天津昌海新材料科技发展有限公司 | Graphene modified high-weather-resistance high-resilience nano polymer joint filling material and preparation method thereof |
| CN110293646A (en) * | 2019-06-10 | 2019-10-01 | 长兴正发热电耐火材料有限公司 | A kind of production technology of lightweight heat-proof joint sealing material |
| CN113462275A (en) * | 2021-06-30 | 2021-10-01 | 海星(深圳)高新技术研发有限公司 | Preparation method of nano coating liquid |
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