CN110511341A - A kind of flame-retardant polyurethane sound absorption and noise reduction material and preparation method thereof - Google Patents
A kind of flame-retardant polyurethane sound absorption and noise reduction material and preparation method thereof Download PDFInfo
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- CN110511341A CN110511341A CN201910815001.4A CN201910815001A CN110511341A CN 110511341 A CN110511341 A CN 110511341A CN 201910815001 A CN201910815001 A CN 201910815001A CN 110511341 A CN110511341 A CN 110511341A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
Abstract
The invention belongs to polymeric material fields, and in particular to a kind of flame-retardant polyurethane sound absorption and noise reduction material and preparation method thereof.The present invention adds fire-retardant filler in the synthesis process of polyurethane, the fire-retardant filler is modified expansible graphite, using a step foaming synthesis of polyurethane foam, the preparation method simple process, molding time is short, and polyurethane foam acoustic absorptivity prepared by the present invention is high, and absorption band is wide, limit oxygen index coefficient is high, good flame retardation effect.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to a kind of flame-retardant polyurethane sound absorption and noise reduction material and its preparation
Method.
Background technique
With modern science and technology, the rapid development of industry, not only the moment affects the normal life and work of people to noise pollution
Make, while the physical and mental health of serious damage people.Noise problem is on the rise, and how effectively to have taken precautions against and control noise problem
The a great problem urgently to be resolved as today's society, the propagation of sound are by three source of students, route of transmission and recipient part groups
At control sound source is to handle the first step of noise pollution, but the objective reality due to sound source in the environment, so people focus on
Harm of the noise to recipient is reduced by controlling the route of transmission of noise.Therefore develop a kind of sound-absorbing material then at
The feasibility direction of field of noise control.
Sound-absorbing material is the material with stronger absorption sound energy, reducing noise performance.Porosity, film by means of itself
Effect or resonant interaction and can have the material of absorption to incident sound, one of the original part of ultrasonography equipment.Absorb sound material
Material will be matched with the acoustic characteristic impedance of the sound bearing medium of surrounding, enter sound-absorbing material with enabling sound areflexia, and enable incident sound
The overwhelming majority is absorbed.Sound is derived from object earthquake motion, it causes the vibration for closing on air and forms sound wave, and in air dielectric
In propagate around.When sound is passed to sound-absorbing material surface, sound a part of can be reflected, and a part of penetrable material, there are also one
Partially due to You Shengneng is converted to thermal energy, sound energy with surrounding medium friction when the vibration of sound-absorbing material or sound are propagated wherein
It is depleted, i.e., usually said sound is absorbed by material.The one kind of porous material as sound-absorbing material, physical structure are characterized in material
Material is internal a large amount of, interpenetrating, outwardly open micropore, i.e. material has certain gas permeability.Sound-absorbing porous material
Sound absorbing mechanism be to cause the air vibration in hole when sound wave incident is to porous material.It is viscous with air due to rubbing
Resistance enables a part of sound to be transformed into thermal energy；In addition, the heat transfer between air and hole wall, fiber in hole, can also cause
Heat loss makes sound energy attenuation.
Polyurethane foam can be very good absorption of noise as a kind of porous material with excellent sound absorption performance, it
Application range also very extensively, almost penetrate into each department of national economy, especially furniture, bed accessory, transport, refrigeration,
The departments such as building use very universal, it has also become one of indispensable material.But polyurethane foam be also it is a kind of inflammable and
Burning can generate the material of harmful substance, and flame retardant property is in urgent need to be improved.
Summary of the invention
The present invention in view of the deficiencies of the prior art, and it is an object of the present invention to provide a kind of flame-retardant polyurethane sound absorption and noise reduction material and its
Preparation method.
For achieving the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, which comprises the steps of:
(1) preparation of modified expansible graphite: expansible graphite is modified using phosphorus oxychloride, 1,4- dioxane
Obtain modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. the formula of flame-retardant polyurethane includes white material and black material, each group distribution ratio of the white material are as follows: polyether polyol,
Catalyst a, catalyst b, activating agent, foaming agent, modified expansible graphite；The black material is isocyanates；
B. polyether polyol is placed in glass beaker, sequentially add in sequence catalyst a, catalyst b, foaming agent,
Activating agent after mechanical stirring is uniform at a certain temperature, adds modified expansible graphite, mechanical stirring is equal under certain temperature
White material is obtained after even；Then black material is added in white material, is poured into open mold rapidly after stirring, to frostproof froth n to certain height
Degree, which is put into baking oven, to be cured to get flame-retardant polyurethane sound absorption and noise reduction material is arrived.
In above scheme, the dosage of the phosphorus oxychloride is the 6~9% of polyether polyol quality, the Isosorbide-5-Nitrae-dioxy six
The dosage of ring is the 150~180% of polyether polyol quality, and the dosage of the expansible graphite is the 5 of polyether polyol quality
~25%.
In above scheme, each component ratio of the white material are as follows: polyether polyol 100~150 parts by weight, catalyst a
Dosage accounts for the 0.2~0.5% of the dosage polyether polyol quality of the 0.2~0.9% of polyether polyol quality, catalyst b, activity
The dosage that the dosage of agent accounts for the 0.5~2% of polyether polyol quality, foaming agent accounts for 1~5 % of polyether polyol quality, changes
The dosage of property expansible graphite accounts for the 5~20% of polyether polyol quality.
In above scheme, the dosage of the isocyanates accounts for the 35~55% of polyether polyol quality.
In above scheme, 10~22min is stirred at a temperature of 35~40 DEG C；Modified expansible graphite is added, 65~
4~8h is stirred at a temperature of 75 DEG C.
In above scheme, the temperature of the curing is 45~70 DEG C, and the time of the curing is 30~75min.
Beneficial effects of the present invention: the present invention adds fire-retardant filler in the synthesis process of polyurethane, is foamed using a step
Method synthesis of polyurethane foam, simple process, molding time are short；Prepared polyurethane foam acoustic absorptivity is high, and absorption band is wide,
Limit oxygen index coefficient is high, good flame retardation effect.
Detailed description of the invention
Fig. 1 is the sound absorbing performance of flame-retardant polyurethane sound absorption and noise reduction material prepared in embodiment 1,2,3,4,5.
Fig. 2 is the limit oxygen index system of flame-retardant polyurethane sound absorption and noise reduction material prepared in embodiment 1,2,3,4,5
Number.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
The measurement of the limit oxygen index of heretofore described fire-retardant sound-absorbing material is according to GB/T2406-1993 " Plastics Combustion
Method for testing performance oxygen index method " it provides to be measured.
Embodiment 1
A kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, includes the following steps:
(1) preparation of modified expansible graphite: expansible graphite 5g, phosphorus oxychloride 6g, Isosorbide-5-Nitrae-dioxane 150g, successively
Isosorbide-5-Nitrae-dioxane, expansible graphite, phosphorus oxychloride are added in three-necked flask, 60 DEG C of heating water bath 6h, filtering drying obtains
Modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. white material: polyether polyol 100g, triethylene diamine (catalyst a) 0.8g, dibutyl tin dilaurate (catalyst b)
0.4g, water (foaming agent) 3g, silicone oil (activating agent) 2g；Black material: isocyanates 46.4g；
B. polyether polyol is placed in glass beaker, sequentially adds triethylene diamine, two fourth of tin dilaurate in sequence
Tin, water, silicone oil, mechanical stirring 16min under 40 DEG C of heating water baths, add modified expansible graphite, machine under 65 DEG C of heating water baths
Tool stirs 4h, obtains white material after mixing evenly；Then it pours into open mold rapidly after black material stirring 2min is added, is sent out to foam
It steeps to be put into 50 DEG C of baking ovens after 30mm high and cures 60min, obtain flame-retardant polyurethane sound absorption and noise reduction material.
Effect assessment: the sound absorbing performance that the present embodiment prepares obtained flame-retardant type polyurethane sound absorption and noise reduction material is shown in Fig. 1, Fig. 1
It has been shown that, average sound absorption coefficient are higher than 0.57, and the acoustic absorptivity of low frequency absorption peak is up to 0.61, and the acoustic absorptivity at high-frequency absorption peak is high
Up to 0.82, limit oxygen index coefficient is shown in Fig. 2, and limit oxygen index value reaches 20.3%.
Embodiment 2
A kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, includes the following steps:
(1) preparation of modified expansible graphite: expansible graphite 13g, phosphorus oxychloride 10.4g, Isosorbide-5-Nitrae-dioxane 221g,
Successively Isosorbide-5-Nitrae-dioxane, expansible graphite, phosphorus oxychloride are added in three-necked flask, 55 DEG C of heating water bath 5.5h, filtering is dried
It is dry to obtain modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. white material: polyether polyol 130g, triethylene diamine (catalyst a) 0.65g, dibutyl tin dilaurate (catalyst
B) 0.26g, water (foaming agent) 6.5g, silicone oil (activating agent) 2.6g；Black material: isocyanates 64.48g；
B. polyether polyol is placed in glass beaker, sequentially adds triethylene diamine, two fourth of tin dilaurate in sequence
Tin, water, silicone oil, mechanical stirring 16min under 40 DEG C of heating water baths, add modified expansible graphite, machine under 65 DEG C of heating water baths
Tool stirs 4h, obtains white material after mixing evenly；Then it pours into open mold rapidly after black material stirring 2min is added, is sent out to foam
It steeps to be put into 50 DEG C of baking ovens after 30mm high and cures 60min, obtain flame-retardant polyurethane sound absorption and noise reduction material.
Effect assessment: the sound absorbing performance that the present embodiment prepares obtained flame-retardant type polyurethane sound absorption and noise reduction material is shown in Fig. 1, Fig. 1
It has been shown that, average sound absorption coefficient are higher than 0.52, and the acoustic absorptivity of low frequency absorption peak is up to 0.62, and the acoustic absorptivity at high-frequency absorption peak is high
Up to 0.72, limit oxygen index coefficient is shown in Fig. 2, and limit oxygen index value reaches 21.7%.
Embodiment 3
A kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, includes the following steps:
(1) preparation of modified expansible graphite: expansible graphite 22.5g, phosphorus oxychloride 13.5g, 1,4- dioxane
270g successively Isosorbide-5-Nitrae-dioxane, expansible graphite, phosphorus oxychloride is added in three-necked flask, 45 DEG C of heating water bath 7h, filtering
Drying obtains modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. white material: polyether polyol 150g, triethylene diamine (catalyst a) 1.35g, dibutyl tin dilaurate (catalyst
B) 0.3g, water (foaming agent) 6g, silicone oil (activating agent) 3g；Black material: isocyanates 67.2g；
B. polyether polyol is placed in glass beaker, sequentially adds triethylene diamine, two fourth of tin dilaurate in sequence
Tin, water, silicone oil, mechanical stirring 20min under 35 DEG C of heating water baths, add modified expansible graphite, machine under 70 DEG C of heating water baths
Tool stirs 8h, obtains white material after mixing evenly；Then it pours into open mold rapidly after black material stirring 2min is added, is sent out to foam
It steeps to be put into 65 DEG C of baking ovens after 30mm high and cures 70min, obtain flame-retardant polyurethane sound absorption and noise reduction material.
Effect assessment: the sound absorbing performance that the present embodiment prepares obtained flame-retardant type polyurethane sound absorption and noise reduction material is shown in Fig. 1, Fig. 1
It has been shown that, average sound absorption coefficient are higher than 0.60, and the acoustic absorptivity of low frequency absorption peak is up to 0.65, and the acoustic absorptivity at high-frequency absorption peak is high
Up to 0.82, limit oxygen index coefficient is shown in Fig. 2, and limit oxygen index value reaches 23.3%.
Embodiment 4
A kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, includes the following steps:
(1) preparation of modified expansible graphite: expansible graphite 27g, phosphorus oxychloride 9.45g, 1,4- dioxane
22.75g successively Isosorbide-5-Nitrae-dioxane, expansible graphite, phosphorus oxychloride is added in three-necked flask, 50 DEG C of heating water bath 6h, mistake
Filter drying obtains modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. white material: polyether polyol 135g, triethylene diamine (catalyst a) 0.945g, dibutyl tin dilaurate (catalyst
B) 0.405g, water (foaming agent) 2.7g, silicone oil (activating agent) 2.7g；Black material: isocyanates 64.125g；
B. polyether polyol is placed in glass beaker, sequentially adds triethylene diamine, two fourth of tin dilaurate in sequence
Tin, water, silicone oil, mechanical stirring 14min under 37 DEG C of heating water baths, add modified expansible graphite, machine under 68 DEG C of heating water baths
Tool stirs 6.5h, obtains white material after mixing evenly；Then it is poured into open mold rapidly after black material stirring 3min is added, to foam
It is put into after foaming to 30mm high in 45 DEG C of baking ovens and cures 75min, obtain flame-retardant polyurethane sound absorption and noise reduction material.
Effect assessment: the sound absorbing performance that the present embodiment prepares obtained flame-retardant type polyurethane sound absorption and noise reduction material is shown in Fig. 1, Fig. 1
It has been shown that, average sound absorption coefficient are higher than 0.75, and the acoustic absorptivity of low frequency absorption peak is up to 0.68, and the acoustic absorptivity at high-frequency absorption peak is high
Up to 0.90, limit oxygen index coefficient is shown in Fig. 2, and limit oxygen index value reaches 24.2%.
Embodiment 5
A kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, includes the following steps:
(1) preparation of modified expansible graphite: expansible graphite 35g, phosphorus oxychloride 11.2g, Isosorbide-5-Nitrae-dioxane 245g,
Successively Isosorbide-5-Nitrae-dioxane, expansible graphite, phosphorus oxychloride are added in three-necked flask, 45 DEG C of heating water bath 7.5h, filtering is dried
It is dry to obtain modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. white material: polyether polyol 140g, triethylene diamine (catalyst a) 0.7g, dibutyl tin dilaurate (catalyst b)
0.56g, water (foaming agent) 2.8g, silicone oil (activating agent) 2.8g；Black material: isocyanates 68.6g；
B. polyether polyol is placed in glass beaker, sequentially adds triethylene diamine, two fourth of tin dilaurate in sequence
Tin, water, silicone oil, mechanical stirring 22min under 37 DEG C of heating water baths, add modified expansible graphite, machine under 72 DEG C of heating water baths
Tool stirs 8h, obtains white material after mixing evenly；Then it is poured into open mold rapidly after black material stirring 2.5min is added, to foam
It is put into after foaming to 30mm high in 55 DEG C of baking ovens and cures 75min, obtain flame-retardant polyurethane sound absorption and noise reduction material.
Effect assessment: the sound absorbing performance that the present embodiment prepares obtained flame-retardant type polyurethane sound absorption and noise reduction material is shown in Fig. 1, Fig. 1
It has been shown that, average sound absorption coefficient are higher than 0.68, and the acoustic absorptivity of low frequency absorption peak is up to 0.63, and the acoustic absorptivity at high-frequency absorption peak is high
Up to 0.71, limit oxygen index coefficient is shown in Fig. 2, and limit oxygen index value reaches 25.7%.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and is not the limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection scope of the invention.
Claims (6)
1. a kind of preparation method of flame-retardant polyurethane sound absorption and noise reduction material, which comprises the steps of:
(1) preparation of modified expansible graphite: expansible graphite is modified to obtain using phosphorus oxychloride, 1,4- dioxane
Modified expansible graphite；
(2) preparation of flame-retardant polyurethane sound absorption and noise reduction material:
A. the formula of flame-retardant polyurethane includes white material and black material, each group distribution ratio of the white material are as follows: polyether polyol is urged
Agent a, catalyst b, activating agent, foaming agent, modified expansible graphite；The black material is isocyanates；
B. polyether polyol is placed in glass beaker, sequentially adds catalyst a, catalyst b, foaming agent, work in sequence
Property agent, after mechanical stirring is uniform at a certain temperature, adds modified expansible graphite, mechanical stirring is uniform under certain temperature
After obtain white material；Then black material is added in white material, is poured into open mold rapidly after stirring, to frostproof froth n to certain altitude
It is put into baking oven and cures to get flame-retardant polyurethane sound absorption and noise reduction material is arrived.
2. preparation method according to claim 1, which is characterized in that the dosage of phosphorus oxychloride described in step (1) accounts for poly-
The 6 ~ 9% of ethoxylated polyhydric alcohol quality, the dosage of the Isosorbide-5-Nitrae-dioxane account for the 150 ~ 180% of polyether polyol quality, it is described can be swollen
The dosage of swollen graphite accounts for the 5 ~ 25% of polyether polyol quality.
3. preparation method according to claim 1, which is characterized in that the dosage of each component of the white material are as follows: polyether polyols
The dosage that 100 ~ 150 parts by weight of alcohol, the dosage of catalyst a account for the 0.2 ~ 0.9% of polyether polyol quality, catalyst b accounts for polyethers
The 0.2 ~ 0.5% of polyol quality, the dosage that the dosage of activating agent accounts for the 0.5 ~ 2% of polyether polyol quality, foaming agent accounts for polyethers
The 1 ~ 5% of polyol quality, the dosage of modified expansible graphite accounts for polyether polyol quality 5 ~ 20%.
4. preparation method according to claim 1, which is characterized in that the dosage of the isocyanates accounts for polyether polyol matter
The 35 ~ 55% of amount.
5. preparation method according to claim 1, which is characterized in that stir 10 ~ 22min at a temperature of 35 ~ 40 DEG C；Again plus
Enter modified expansible graphite, 4 ~ 8h is stirred at a temperature of 65 ~ 75 DEG C.
6. preparation method according to claim 1, which is characterized in that the temperature of the curing is 45 ~ 70 DEG C, the curing
Time be 30 ~ 75min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112457463A (en) * | 2020-11-20 | 2021-03-09 | 武汉科技大学 | Low-pollution polyurethane foam sound absorption material and preparation method thereof |
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| CN112457463A (en) * | 2020-11-20 | 2021-03-09 | 武汉科技大学 | Low-pollution polyurethane foam sound absorption material and preparation method thereof |
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