CN101812229B - Heat-insulating and shock-absorbing protective film and preparation method thereof - Google Patents
Heat-insulating and shock-absorbing protective film and preparation method thereof Download PDFInfo
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- CN101812229B CN101812229B CN201010146176XA CN201010146176A CN101812229B CN 101812229 B CN101812229 B CN 101812229B CN 201010146176X A CN201010146176X A CN 201010146176XA CN 201010146176 A CN201010146176 A CN 201010146176A CN 101812229 B CN101812229 B CN 101812229B
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- chainextender
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- Treatment And Processing Of Natural Fur Or Leather (AREA)
- Paints Or Removers (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
Abstract
The invention relates to a heat-insulating and shock-absorbing protective film which is prepared by polymerizing polyester glycol and isocyanate, carrying out chain extending reaction under the action of a catalyst, coating on a flat release paper by batch with a drying PU production process and foaming. The protective film has excellent heat-insulating performance and shock resistance and is suitable for inner linings of clothing for spacecrafts, vehicles and field high-cold operation and places having special requirements on heat insulation and shock absorption.
Description
Technical field
The present invention relates to a kind of heat insulation protective film; Be applicable to that spacecraft, vehicle, open-air high and cold operation have the occasion of particular requirement with the dress ornament liner with to heat-insulating and shock-absorbing; Be particularly useful for the heat-insulating and shock-absorbing protection of aircraft aerial main cabin emergency pressure relief and service door open system, the method for manufacture of this heat-insulating and shock-absorbing protective film is provided simultaneously.
Background technology
At present, in the aerial main cabin emergency pressure relief and service door open system of aircraft, all do not see the report that heat-insulating and shock-absorbing protective film is arranged both at home and abroad.
In recent years; Our company is devoted to the exploitation that synthetic leather is covered with paint, lacquer, colour wash, etc. resin; With polyester glycol or polyether glycol and isocyanic ester in the presence of catalyzer, chainextender; Generate aromatic series or aliphatics Waterproof Breathable synthetic leather covering with paint resin with pre-polymerization or half pre-polymerization method of manufacture, the product waterproof effect is obvious, steady quality.
" high hydrolysis resistance, weatherability leather imitation resin for synthetic leather and method of manufacture thereof " (2007100197306) of our company's application disclose a kind of its water-resistant capacity and have reached the imitation leather resin of life-time service 5-10 level out of doors; By molecular weight is that 2000 polyester glycol, isocyanic ester carry out prepolymerization reaction and get under catalyzer (dibutyl tin laurate or organo-bismuth), chainextender (terepthaloyl moietie or 1,4 butyleneglycol) effect.This resin characteristics is high hydrolytic resistance and weather resistance, if produce heat-insulating and shock-absorbing protective film with it, its heat-insulating and shock-absorbing performance is undesirable.
Summary of the invention
Invention is just in order to overcome above-mentioned deficiency; Enterprising row is perfect on 2007100197306 disclosed imitation leather resin bases; Develop a kind of spacecraft, vehicle, open-air high and cold operation of being applicable to dress ornament liner and the heat-insulating and shock-absorbing protective film that has the occasion of particular requirement to use to heat-insulating and shock-absorbing; Main innovation is to adjust component materials compatibility and ratio, adds filled with foaming material, adopts PU synthetic leather dry method masking technique to make again.Specifically implement like this:
Heat-insulating and shock-absorbing protective film is characterized in that the weight proportion that raw material is formed is:
Polyester glycol compsn 45-60%
Isocyanic ester MDI 40-55%
Described polyester glycol compsn is that molecular weight is that 2000 polyester glycol and molecular weight are 1000 polyester glycol with weight ratio 2-3: 1 mixes.
With polyester glycol compsn and isocyanic ester MDI mixture is benchmark for 100 parts, outer again the adding:
The phosphoric acid trace is transferred pH value 4.0-5.0
Chainextender terepthaloyl moietie or 1,4 butyleneglycol 5-10%
NN-N 250-400%
Organo-bismuth 0.02-0.05%
Methyl alcohol 0.2-0.5%
Toluene 100-200%
Butanone 150-300%
Aerosil 2-6%
Cellmic C 121 3-5%
Organosilicon 0.2-0.5%
Adopt aerosil as filler among the present invention, not only resistance toheat is good, and can let uniform in foaming soft, good film-forming property.
Make spent glycol or 1.4 butyleneglycols make chainextender among the present invention, the organo-bismuth that adopts environmental protection is as catalyzer, and is safer, more environmental protection.
Cellmic C 121 is a kind of AC whipping agent, and organosilicon is peeled off auxiliary agent.
The method of manufacture of this heat-insulating and shock-absorbing protective film is, is that 2000 and 1000 polyester glycol compsn, isocyanic ester MDI transfer pH value 4-5 with micro-phosphoric acid with molecular weight by weight ratio, drops into the catalyzer organo-bismuth; Being warming up to 75 ℃-80 ℃ carried out prepolymerization reaction 1-1.5 hour; Be cooled to 50 ℃-55 ℃ again, dilute, drop into chainextender more in batches with the 10-20% of NN-N weight; Increase according to viscosity; In reaction process, progressively drop into remaining solvent NN-N, to 10-13 ten thousand CP.S, drop into the methyl alcohol termination reaction until reaction viscosity; Be warmed up to again 60 ℃-70 ℃ insulation reaction 0.5-1 hour, be cooled under 50 ℃, drop into toluene, butanone, aerosil, Cellmic C 121, organosilicon successively and mix, viscosimetric discharging during to 3-5 ten thousand CP.S; Adopt PU synthetic leather dry method leather-making technology, in batches discharging is coated on the dull and stereotyped separate-type paper, under 155 ℃-170 ℃, carry out foaming treatment, process dry film.
In this method of manufacture, the catalyzer organo-bismuth divides secondary to add, and the 60-70% of the weight organo-bismuth gross weight that adds for the first time after polyreaction 40-60 minute, adds remaining organo-bismuth again.
Adopt chain extension method in batches in this method of manufacture; Usually chainextender is above in three batches drops into, and the best drops in four batches, except that last; The input weight of each batch chainextender is the 40-50% that last time drops into the back surplus, and last chainextender input adopts the mode that slowly splashes into.
Remaining solvent NN-N begins progressively to add dropping into chainextender for the second time in this method of manufacture.
The present invention is with polyester glycol and isocyanic ester polymerization; Under the effect of catalyzer, carry out chain extending reaction, adopt dry method PU production technique then, get through foaming in dull and stereotyped separate-type paper on batch coating; Have good heat-proof quality and shake-proof ability; " the big aircraft of ARJ21-700 aerial main cabin emergency pressure relief and the service door open system " that this product has been used for developing, and on 101 sorties that be installed in the ARJ21-700 aircraft in October, 2009 were taken a flight test machine, steady quality was reliable.
Embodiment
Embodiment 1, and the mixed polyester glycol (2000 and 1000 molecular weight are 2: 1) in 50 parts of molecular weight 2000 and 1000 among 50 parts of isocyanic ester MDI, is transferred pH value 4 with micro-phosphoric acid; Drop into 0.021 part of catalyzer organo-bismuth, be warming up to 75 ℃ of reactions 60 minutes, add 0.009 part of remaining organo-bismuth again; React half a hour, be cooled to 55 ℃ of input NN-N (DMF) 50 parts and dilute, drop into totally 5 parts of chainextender terepthaloyl moietie (MEG) in three batches; First drops into 2.5 parts, and second batch is dropped into 1.25 parts, drops into 50 parts of solvent NN-Ns; The 3rd batch slowly splashes into remaining terepthaloyl moietie, and the reaction medium viscosity constantly rises, and progressively adds 150 parts of solvent DMF according to the viscosity growth pattern; Viscosity sharply rises, and viscosimetric to 12.5 ten thousand CP.S drop into 0.45 part of termination reaction agent methyl alcohol immediately; Be warmed up to 60 ℃ of insulation reaction and be cooled to 48 ℃ in 0.6 hour again; Drop into 4 parts of 200 parts of 140 parts of toluene, butanone, aerosils, 3.5 parts of AC whipping agent Cellmic C 121s in the prescription successively, peel off 0.3 part of auxiliary agent organosilicon, viscosimetric to 3.8 ten thousand CP.S dischargings packing; Adopt PU synthetic leather dry method leather-making technology then, time be coated on the dull and stereotyped separate-type paper in three batches, under 155 ℃-170 ℃ of oven temperatures, carry out foaming treatment, process dry film.
Embodiment 2, and the mixed polyester glycol (2000 and 1000 molecular weight are 3: 1) in 45 parts of molecular weight 2000 and 1000 among 55 parts of isocyanic ester MDI, is transferred pH value 4.8 with micro-phosphoric acid; Drop into 0.013 part of catalyzer organo-bismuth, be warming up to 78 ℃ of reactions 40 minutes, add 0.007 part of remaining organo-bismuth again, react after 20 minutes; Be cooled to 52 ℃ of input solvent NN-Ns again and dilute for 60 parts, drop into 10 parts of chainextender 1,4 butyleneglycols in four batches, first drops into 1; 5 parts of 4 butyleneglycols, second batch is dropped into 2 parts of 1,4 butyleneglycols; Drop into 100 parts of NN-Ns, the 3rd batch is dropped into 1.4 parts of 1,4 butyleneglycols; Progressively add 100 parts of solvent NN-Ns according to the viscosity growth pattern, the 4th batch of beginning slowly splashes into 1,4 remaining butyleneglycol; Drop into 140 parts of remaining NN-Ns, viscosimetric reaches 130,000 CP.S, drops into 0.5 part of termination reaction agent methyl alcohol; Being warmed up to 67 ℃ of insulation reaction was cooled to 50 ℃ in 1 hour again and drops into down 6 parts of 300 parts of 200 parts of toluene, butanone, aerosils, 5 parts of AC whipping agent Cellmic C 121s in the prescription, peels off 0.5 part of auxiliary agent organosilicon, viscosimetric to 5 ten thousand CP.S dischargings packing; Adopt PU synthetic leather dry method leather-making technology then, divide two batches of friendships to be coated on the dull and stereotyped separate-type paper, under 155 ℃-170 ℃ of oven temperatures, carry out foaming treatment, process dry film.
Embodiment 3, and the mixed polyester glycol (2000 and 1000 molecular weight are 2.5: 1) in 60 parts of molecular weight 2000 and 1000 is among 40 parts of isocyanic ester MDI; Transfer pH value 5 with micro-phosphoric acid, drop into 0.03 part of catalyzer organo-bismuth, be warming up to 80 ℃ of reactions 50 minutes; Add 0.02 part of remaining organo-bismuth again, react half a hour, be cooled to 50 ℃ of input NN-N (DMF) 36 parts and dilute; Drop into totally 7 parts of terepthaloyl moietie (MEG) in four batches, first drops into 3 parts, and second batch is dropped into 2 parts; Drop into thinner NN-N DMF80 part, the 3rd batch is dropped into 1 part of chainextender, drops into solvent NN-N DMF90 part with the viscosity growth pattern; The 4th batch slowly splashes into remaining terepthaloyl moietie, and the reaction medium viscosity constantly rises, and adds solvent NN-N DMF154 part again; Viscosity sharply rises, and viscosimetric to 10 ten thousand CP.S drop into 0.2 part of termination reaction agent methyl alcohol immediately; Be warmed up to 70 ℃ of insulation reaction and be cooled to 45 ℃ in 0.5 hour again; Drop into 2 parts of 150 parts of 100 parts of toluene, butanone, aerosils, 3 parts of AC whipping agent Cellmic C 121s in the prescription successively, peel off 0.2 part of auxiliary agent organosilicon, viscosimetric to 3 ten thousand CP.S dischargings packing; Adopt PU synthetic leather dry method leather-making technology then, time be coated on the dull and stereotyped separate-type paper in three batches, under 155 ℃-170 ℃ of oven temperatures, carry out foaming treatment, process dry film.
It is following that embodiment makes the performance of products parameter index:
Claims (7)
1. heat-insulating and shock-absorbing protective film is characterized in that the weight proportion that raw material is formed is:
Polyester glycol compsn 45-60%
Isocyanic ester MDI 40-55%
Described polyester glycol compsn is that molecular weight is that 2000 polyester glycol and molecular weight are 1000 polyester glycol with weight ratio 2-3: 1 mixes,
With polyester glycol compsn and isocyanic ester MDI mixture is benchmark for 100 parts, outer again the adding:
The pH value that the phosphoric acid trace telomerizes esterdiol compsn and isocyanic ester MDI mixture is 4.0-5.0
2. the method for manufacture of heat-insulating and shock-absorbing protective film is characterized in that be that 2000 and 1000 polyester glycol compsn, isocyanic ester MDI transfer pH value 4-5 with micro-phosphoric acid by the described weight proportion of claim 1 with molecular weight, drops into the catalyzer organo-bismuth; Being warming up to 75 ℃-80 ℃ carried out prepolymerization reaction 1-1.5 hour; Be cooled to 50 ℃-55 ℃ again, dilute, drop into chainextender more in batches with the 10-20% of NN-N weight; Increase according to viscosity; In reaction process, progressively drop into remaining solvent NN-N, to 10-13 ten thousand CP.S, drop into the methyl alcohol termination reaction until reaction viscosity; Be warmed up to again 60 ℃-70 ℃ insulation reaction 0.5-1 hour, be cooled under 50 ℃, drop into toluene, butanone, aerosil, Cellmic C 121, organosilicon successively and mix, viscosimetric discharging during to 3-5 ten thousand CP.S; Adopt PU synthetic leather dry method leather-making technology, in batches discharging is coated on the dull and stereotyped separate-type paper, under 155 ℃-170 ℃, carry out foaming treatment, process dry film.
3. method of manufacture according to claim 2 is characterized in that the catalyzer organo-bismuth divides secondary to add, and the weight that adds for the first time is the 60-70% of organo-bismuth gross weight, after polyreaction 40-60 minute, adds remaining organo-bismuth again.
4. method of manufacture according to claim 2 is characterized in that the above in three batches input of chainextender, and except that last, input weight of each batch chainextender is the 40-50% that last time drops into the back surplus.
5. method of manufacture according to claim 4 is characterized in that chainextender drops in four batches.
6. according to claim 2,4, one of 5 described method of manufacture, it is characterized in that last chainextender input adopts the mode that slowly splashes into.
7. method of manufacture according to claim 2 is characterized in that remaining solvent NN-N drops into chainextender in the second time and begins progressively to add.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010146176XA CN101812229B (en) | 2010-04-02 | 2010-04-02 | Heat-insulating and shock-absorbing protective film and preparation method thereof |
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| CN201010146176XA CN101812229B (en) | 2010-04-02 | 2010-04-02 | Heat-insulating and shock-absorbing protective film and preparation method thereof |
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| CN101812229A CN101812229A (en) | 2010-08-25 |
| CN101812229B true CN101812229B (en) | 2012-06-20 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013086217A (en) * | 2011-10-19 | 2013-05-13 | Dic Corp | Urethane resin composition for polishing pad, polyurethane polishing pad, and method of manufacturing polyurethane polishing pad |
| CN102582304A (en) * | 2012-03-01 | 2012-07-18 | 杭州鹰自达塑业有限公司 | Method for forming foaming product on release paper by adopting printing technology |
| CN110306352A (en) * | 2019-07-30 | 2019-10-08 | 浙江百得利制革有限公司 | A kind of preparation process of double-face leather clothing leather |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092538A (en) * | 2006-06-23 | 2007-12-26 | 宜兴环保科技工业园新光化工厂 | Waterproof, humidity permeable resin in aliphatic series for overcoating synthetic leather, manufactureing method of half-advanced polymerization |
| CN101092537A (en) * | 2006-06-23 | 2007-12-26 | 宜兴环保科技工业园新光化工厂 | Waterproof, humidity permeable resin in aromatic for overcoating synthetic leather, manufactureing method of half-advanced polymerization |
| CN101092536A (en) * | 2006-06-23 | 2007-12-26 | 宜兴环保科技工业园新光化工厂 | Waterproof, humidity permeable resin in aromatic for overcoating synthetic leather, and fabricating method |
| CN101240054A (en) * | 2007-02-08 | 2008-08-13 | 宜兴环保科技工业园新光化工厂 | High hydrolysis resistance and weatherability leather imitation resin for synthetic leather and preparation method thereof |
| US20090286950A1 (en) * | 2008-05-13 | 2009-11-19 | Tesa Ag | Hotmelt process for producing a chemically crosslinked polyurethane film |
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2010
- 2010-04-02 CN CN201010146176XA patent/CN101812229B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092538A (en) * | 2006-06-23 | 2007-12-26 | 宜兴环保科技工业园新光化工厂 | Waterproof, humidity permeable resin in aliphatic series for overcoating synthetic leather, manufactureing method of half-advanced polymerization |
| CN101092537A (en) * | 2006-06-23 | 2007-12-26 | 宜兴环保科技工业园新光化工厂 | Waterproof, humidity permeable resin in aromatic for overcoating synthetic leather, manufactureing method of half-advanced polymerization |
| CN101092536A (en) * | 2006-06-23 | 2007-12-26 | 宜兴环保科技工业园新光化工厂 | Waterproof, humidity permeable resin in aromatic for overcoating synthetic leather, and fabricating method |
| CN101240054A (en) * | 2007-02-08 | 2008-08-13 | 宜兴环保科技工业园新光化工厂 | High hydrolysis resistance and weatherability leather imitation resin for synthetic leather and preparation method thereof |
| US20090286950A1 (en) * | 2008-05-13 | 2009-11-19 | Tesa Ag | Hotmelt process for producing a chemically crosslinked polyurethane film |
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| CN101812229A (en) | 2010-08-25 |
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Granted publication date: 20120620 Termination date: 20160402 |