CN106977829B - A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material - Google Patents
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material Download PDFInfo
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- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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Abstract
The invention discloses a kind of preparation methods of sol deposition hollow polystyrene building thermal insulation material, the present invention will be blended after hollow sol deposition pearl filler epoxidation with amination styrene monomer, it participates in the polymerization reaction of styrene, effectively raise compatibility of the filler between polymer, reunion is effectively reduced, the stability_intensity of finished-product material is improved.Composite material of the invention has good fire-retardant, heat preservation, anti-corrosion, stability_intensity etc., and light weight, and the feature of environmental protection is good, and comprehensive performance is superior.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of preparation of sol deposition hollow polystyrene building thermal insulation material
Method.
Background technique
Polystyrene foamed material is that the auxiliary materials such as foaming agent, heated hair is added using polystyrene resin as base-material
Light material made of bubble.It is with light, thermal coefficient is small, water absorption rate is low, water-fast, ageing-resistant, low temperature resistant, easy processing, valence
The advantages that honest and clean of fine quality, but polystyrene foam heat insulation material is while bringing huge facilitate to people's lives, it is inflammable
Property also to it application bring certain limitation.Polystyrene foam itself is combustible material, under fire and hot conditions
It easily decomposes burning,
And it is generated with a large amount of poison gases.Therefore, it is badly in need of in terms of carrying out to polystyrene foam heat insulation material fire safety
Research work；
The purposes of foamed polystyrene resin is very extensive, since it has high intensity, light weight, splendid heat preservation insulation
Performance and high-selenium corn energy ability, may be used as various instrument, valuables, precision instrument, vegetable and fruit and aquatic products etc.
Packaging material；And because it is low with pyroconductivity, water imbibition is small, electrical insulating property is good, sound insulation, moisture-proof and moulding process are simple
Equal good characteristics, and the roadbed for being widely used in road and bridge is laid with and catches and refrigerate industry with building construction and fishery
Thermal insulation material etc..Wherein, as a kind of excellent construction material, foamed polystyrene resin is mainly used for the room of building
Face and wall have very good energy-saving effect as external heat insulating composite wall；And as heat insulation house surface be suitable for house,
Factory, flat and pitch roofing, the effects of sound insulation, water blocking steam, sealing and insulation can be played.As heat preservation for building
Material, several performance indicators of overriding concern are low thermal conductivity, high fire retardancy, preferable self-strength；
Currently, in order to improve the performances such as the fire-retardant of thermal insulation material, self-strength, heat preservation, it will usually introduce inorganic filler, so
And the compatibility of inorganic filler and polymeric matrix is poor, and the stability of finished product is easy to cause to reduce, and in Conventional insulation
In hollow glass micropearl is often added, there is the thermal insulation property for improving material well, but its higher cost, and be easy
Fragmentation.
Summary of the invention
It is an object of the invention to the poor, cost for the compatibility of inorganic filler and polymeric matrix in the prior art compared with
High problem provides a kind of preparation method of sol deposition hollow polystyrene building thermal insulation material.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, comprising the following steps:
(1) terephthalaldehyde of 1-2 parts by weight, the methyl methacrylate mixing of 20-27 parts by weight are taken, is stirred evenly,
The methanol of mixture weight 30-40% is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, kept the temperature at 60-70 DEG C
40-50 minutes, obtain aldehyde radical monomer；
(2) the initiator mixing for taking above-mentioned aldehyde radical monomer, 0.2-0.4 parts by weight, is added to 6-9 times of mixture weight
It in tetrahydrofuran, is sent in reaction kettle, insulation reaction 6-7 hours at 80-85 DEG C, discharging is cooled to room temperature, vacuum 45-
It is 2-3 hours dry at 50 DEG C, obtain aldehyde radical fluidized polymer；
(3) ethyl orthosilicate for taking 17-20 parts by weight is added in the deionized water of 30-40 times of its weight, stirs 16-
20 minutes, obtain precursor solution；
(4) calcium carbonate for taking 20-30 parts by weight is added in the dehydrated alcohol of 3-4 times of its weight, stirs evenly, and is added
The gamma-aminopropyl-triethoxy-silane of 2-4 parts by weight, ultrasound 20-30 minutes, are distilled off ethyl alcohol, obtain ammonification at 50-60 DEG C
Calcium carbonate；
(5) above-mentioned aldehyde radical fluidized polymer, the mixing of ammonification calcium carbonate are taken, stirs evenly, is added in above-mentioned precursor solution,
The ammonium hydroxide of the 10-13% of 3-5 parts by weight is added dropwise, increasing temperature is 50-60 DEG C, insulated and stirred 2-3 hour, 2700-3000 turn/
Divide under revolving speed and be centrifugated, precipitating is washed, it is 30-40 minutes dry at 70-80 DEG C of vacuum, obtain sol deposition polymer；
(6) above-mentioned sol deposition polymer is added in the acetone of 10-13 times of its weight, is sent to 46-50 DEG C of perseverance
In tepidarium, 10-13 hours are kept the temperature, is discharged, filtering successively washs precipitating acetone, deionized water 2-3 times, air drying,
Obtain hollow sol deposition pearl filler；
(7) above-mentioned hollow sol deposition pearl filler is taken, is added in the dehydrated alcohol of 1.5-2 times of its weight, is added
The epoxychloropropane of 2-3 parts by weight, it is 10-20 minutes ultrasonic, ethyl alcohol is distilled off, obtains the hollow sol deposition calcium carbonate of epoxidation and fills out
Material；
(8) lauryl amine for taking 4-5 parts by weight is added in the dehydrated alcohol of 3-5 times of its weight, stirs evenly, and increases temperature
Degree is 50-60 DEG C, and the styrene of 190-200 parts by weight is added, insulated and stirred 10-20 minutes, obtains amination monomeric polyol liquid；
(9) ammonium persulfate for taking 3-4 parts by weight is added in the deionized water of 60-70 times of its weight, stirs evenly；
(10) the hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, is stirred evenly, is sent into
Into reaction kettle, the stannous octoate that 1-3 parts by weight are added is passed through nitrogen insulated and stirred 20-30 minutes at 40-50 DEG C, is added
Above-mentioned ammonium persulfate aqueous solution, stirs evenly, and adjusting temperature of reaction kettle is 68-71 DEG C, and insulation reaction 4-5 hours, 13-20 is added
The pentane foaming agent of parts by weight, increasing temperature is 110-120 DEG C, keeps the temperature 1-2 hours, cooling discharging, and product is passed through and washs, is dry
It is sent in foaming machine after dry, screening, steam heats 1-2 hours at 0.25-0.3Mpa, 130-140 DEG C, discharging, and room temperature is cold
But to get the sol deposition hollow polystyrene building thermal insulation material.
The initiator is one of azodiisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide.
Advantages of the present invention:
The present invention uses terephthalaldehyde, methyl methacrylate mixing first, aldehyde radical monomer is obtained, then by this list
Body is polymerize under the conditions of initiator, obtains aldehyde radical fluidized polymer, then blended cross linking is carried out with ammonification calcium carbonate, in crosslinking
It is added to simultaneously using ethyl orthosilicate to be dispersed in the sol solutions of presoma by high speed centrifugation, so that silica solution deposits to friendship
The surface of co-product forms the clad of silica solution, and be crosslinked obtained schiff bases has good stabilization under alkaline condition
Property, and the antibacterial antiseptic property of finished product can be improved, sol deposition polymer is added in acetone later, makes polymethyl
Sour methyl esters dissolution removal, obtains the hollow pearl filler of Sol-gel Coated, then by the hollow pearl filler of the Sol-gel Coated
It is handled by epoxidation, is blended, is participated in the polymerization reaction of styrene monomer with amination styrene monomer, using foaming,
Obtain sol deposition hollow polystyrene building thermal insulation material；
Thermal insulation material of the invention contains the hollow pearl filler of Sol-gel Coated, and the filler is light, due to there is silica solution
Cladding protection, be not easily broken, stability is good, and the heat preservation of finished-product material, fire-retardant, mechanical property not only can be improved, also reduce
The weight of finished product, has achieved the effect that lightweight, has been readily transported, installs, reduce production cost, and its cost is relative to hollow
Glass microballoon is lower, can further reduce production cost；
The present invention will be blended after hollow sol deposition pearl filler epoxidation with amination styrene monomer, participate in benzene second
In the polymerization reaction of alkene, compatibility of the filler between polymer is effectively raised, reunion is effectively reduced, improves finished product
The stability_intensity of material.
Composite material of the invention has good fire-retardant, heat preservation, anti-corrosion, stability_intensity etc., and light weight, the feature of environmental protection
Good, comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, comprising the following steps:
(1) terephthalaldehyde of 2 parts by weight, the methyl methacrylate mixing of 27 parts by weight are taken, stirs evenly, is added mixed
The methanol for closing material weight 40%, stirs evenly, is sent in reaction kettle, be passed through nitrogen, keep the temperature 50 minutes at 70 DEG C, obtain aldehyde radical
Change monomer；
(2) the azobisisoheptonitrile mixing for taking above-mentioned aldehyde radical monomer, 0.4 parts by weight, is added to 9 times of mixture weight
It in tetrahydrofuran, is sent in reaction kettle, insulation reaction 7 hours at 85 DEG C, discharges, be cooled to room temperature, done at 50 DEG C of vacuum
Dry 3 hours, obtain aldehyde radical fluidized polymer；
(3) ethyl orthosilicate for taking 20 parts by weight is added in the deionized water of 40 times of its weight, is stirred 20 minutes, is obtained
Precursor solution；
(4) calcium carbonate for taking 30 parts by weight is added in the dehydrated alcohol of 4 times of its weight, stirs evenly, and 4 weight are added
The gamma-aminopropyl-triethoxy-silane of part, ultrasound 30 minutes, are distilled off ethyl alcohol, obtain ammonification calcium carbonate at 60 DEG C；
(5) above-mentioned aldehyde radical fluidized polymer, the mixing of ammonification calcium carbonate are taken, stirs evenly, is added in above-mentioned precursor solution,
The ammonium hydroxide of the 10-13% of 5 parts by weight is added dropwise, increasing temperature is 60 DEG C, insulated and stirred 3 hours, is centrifuged under 3000 revs/min of revolving speeds
Precipitating is washed in separation, 40 minutes dry at 80 DEG C of vacuum, obtains sol deposition polymer；
(6) above-mentioned sol deposition polymer is added in the acetone of 13 times of its weight, is sent to 50 DEG C of water bath with thermostatic control
In, 13 hours are kept the temperature, is discharged, filtering successively washs precipitating acetone, deionized water 2 times, air drying obtains hollow colloidal sol
Deposit pearl filler；
(7) above-mentioned hollow sol deposition pearl filler is taken, is added in the dehydrated alcohol of 2 times of its weight, 2 weight are added
The epoxychloropropane of part, ultrasound 20 minutes, is distilled off ethyl alcohol, obtains the hollow sol deposition pearl filler of epoxidation；
(8) lauryl amine for taking 5 parts by weight is added in the dehydrated alcohol of 5 times of its weight, stirs evenly, and increases temperature and is
60 DEG C, the styrene of 200 parts by weight is added, insulated and stirred 20 minutes, obtains amination monomeric polyol liquid；
(9) ammonium persulfate for taking 4 parts by weight is added in the deionized water of 70 times of its weight, stirs evenly；
(10) the hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, is stirred evenly, is sent into
Into reaction kettle, the stannous octoate of 3 parts by weight is added, insulated and stirred 30 minutes, are passed through nitrogen at 50 DEG C, and above-mentioned over cure is added
Sour aqueous ammonium, stirs evenly, and adjusting temperature of reaction kettle is 68-71 DEG C, and insulation reaction 5 hours, the pentane of 20 parts by weight is added
Foaming agent, increasing temperature is 120 DEG C, keeps the temperature 2 hours, product is sent to hair by cooling discharging after washing, drying, screening
In bubble machine, steam is heated 2 hours at 0.3Mpa, 140 DEG C, discharging, and room temperature is cooling to get the hollow polyphenyl second of the sol deposition
Alkene building thermal insulation material.
Performance test:
The flame retardant properties, mechanical properties of the sol deposition hollow polystyrene building thermal insulation material of the present embodiment 1 tests knot
Fruit shows:
Oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, bending strength 0.27Mpa, compressive strength 0.21Mpa,
Thermal coefficient 0.029w/m.k.
Embodiment 2
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, comprising the following steps:
(1) terephthalaldehyde of 1 parts by weight, the methyl methacrylate mixing of 20 parts by weight are taken, stirs evenly, is added mixed
The methanol for closing material weight 30%, stirs evenly, is sent in reaction kettle, be passed through nitrogen, keep the temperature 40 minutes at 60 DEG C, obtain aldehyde radical
Change monomer；
(2) the azodiisobutyronitrile mixing for taking above-mentioned aldehyde radical monomer, 0.2 parts by weight, is added to 6 times of mixture weight
It in tetrahydrofuran, is sent in reaction kettle, insulation reaction 6 hours at 80 DEG C, discharges, be cooled to room temperature, done at 45 DEG C of vacuum
Dry 2 hours, obtain aldehyde radical fluidized polymer；
(3) ethyl orthosilicate for taking 17 parts by weight is added in the deionized water of 30 times of its weight, is stirred 16 minutes, is obtained
Precursor solution；
(4) calcium carbonate for taking 20 parts by weight is added in the dehydrated alcohol of 3 times of its weight, stirs evenly, and 4 weight are added
The gamma-aminopropyl-triethoxy-silane of part, ultrasound 20 minutes, are distilled off ethyl alcohol, obtain ammonification calcium carbonate at 50 DEG C；
(5) above-mentioned aldehyde radical fluidized polymer, the mixing of ammonification calcium carbonate are taken, stirs evenly, is added in above-mentioned precursor solution,
10% ammonium hydroxide of 3 parts by weight is added dropwise, increasing temperature is 50 DEG C, and insulated and stirred 2 hours, centrifugation divided under 2700 revs/min of revolving speeds
From, precipitating is washed, it is 30 minutes dry at 70 DEG C of vacuum, obtain sol deposition polymer；
(6) above-mentioned sol deposition polymer is added in the acetone of 10 times of its weight, is sent to 46 DEG C of water bath with thermostatic control
In, 10 hours are kept the temperature, is discharged, filtering successively washs precipitating acetone, deionized water 2 times, air drying obtains hollow colloidal sol
Deposit pearl filler；
(7) above-mentioned hollow sol deposition pearl filler is taken, is added in the dehydrated alcohol of 1.5 times of its weight, 2 weights are added
The epoxychloropropane of part is measured, ultrasound 10 minutes is distilled off ethyl alcohol, obtains the hollow sol deposition pearl filler of epoxidation；
(8) lauryl amine for taking 4 parts by weight is added in the dehydrated alcohol of 3 times of its weight, stirs evenly, and increases temperature and is
50 DEG C, the styrene of 190 parts by weight is added, insulated and stirred 10 minutes, obtains amination monomeric polyol liquid；
(9) ammonium persulfate for taking 3 parts by weight is added in the deionized water of 60 times of its weight, stirs evenly；
(10) the hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, is stirred evenly, is sent into
Into reaction kettle, the stannous octoate of 1 parts by weight is added, insulated and stirred 20 minutes, are passed through nitrogen at 40 DEG C, and above-mentioned over cure is added
Sour aqueous ammonium, stirs evenly, and adjusting temperature of reaction kettle is 68 DEG C, and insulation reaction 4 hours, the pentane-blown of 13 parts by weight is added
Agent, increasing temperature is 110 DEG C, keeps the temperature 1 hour, product is sent to foaming machine after washing, drying, screening by cooling discharging
In, steam heats 1 hour at 0.25Mpa, 130 DEG C, discharging, and room temperature is cooling to get the sol deposition hollow polystyrene
Building thermal insulation material.
Performance test:
The flame retardant properties, mechanical properties of the sol deposition hollow polystyrene building thermal insulation material of the present embodiment 2 tests knot
Fruit shows:
Oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, bending strength 0.26Mpa, compressive strength 0.20Mpa,
Thermal coefficient 0.029w/m.k.
Claims (2)
1. a kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, which comprises the following steps:
(1) terephthalaldehyde of 1-2 parts by weight, the methyl methacrylate mixing of 20-27 parts by weight are taken, stirs evenly, is added
The methanol of mixture weight 30-40%, stirs evenly, is sent in reaction kettle, be passed through nitrogen, keeps the temperature 40-50 at 60-70 DEG C
Minute, obtain aldehyde radical monomer；
(2) the initiator mixing for taking above-mentioned aldehyde radical monomer, 0.2-0.4 parts by weight, is added to the tetrahydro of 6-9 times of mixture weight
It in furans, is sent in reaction kettle, insulation reaction 6-7 hours at 80-85 DEG C, discharging is cooled to room temperature, 45-50 DEG C of vacuum
Lower dry 2-3 hours, obtain aldehyde radical fluidized polymer；
(3) ethyl orthosilicate for taking 17-20 parts by weight is added in the deionized water of 30-40 times of its weight, and 16-20 points of stirring
Clock obtains precursor solution；
(4) calcium carbonate for taking 20-30 parts by weight is added in the dehydrated alcohol of 3-4 times of its weight, stirs evenly, and 2-4 weight is added
The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 20-30 minutes, are distilled off ethyl alcohol at 50-60 DEG C, obtain ammonification carbonic acid
Calcium；
(5) above-mentioned aldehyde radical fluidized polymer, the mixing of ammonification calcium carbonate are taken, stirs evenly, is added in above-mentioned precursor solution, be added dropwise
The ammonium hydroxide of the 10-13% of 3-5 parts by weight, increasing temperature is 50-60 DEG C, insulated and stirred 2-3 hours, is turned at 2700-3000 revs/min
The lower centrifuge separation of speed, precipitating is washed, 30-40 minutes dry at 70-80 DEG C of vacuum, obtains sol deposition polymer；
(6) above-mentioned sol deposition polymer is added in the acetone of 10-13 times of its weight, is sent to 46-50 DEG C of thermostatted water
In bath, 10-13 hour are kept the temperature, discharging is filtered, precipitating acetone, deionized water successively washed 2-3 times, air drying, obtained
Empty sol deposition pearl filler；
(7) above-mentioned hollow sol deposition pearl filler is taken, is added in the dehydrated alcohol of 1.5-2 times of its weight, 2-3 weight is added
The epoxychloropropane of part is measured, it is 10-20 minutes ultrasonic, ethyl alcohol is distilled off, obtains the hollow sol deposition pearl filler of epoxidation；
(8) lauryl amine for taking 4-5 parts by weight is added in the dehydrated alcohol of 3-5 times of its weight, stirs evenly, and increases temperature and is
50-60 DEG C, the styrene of 190-200 parts by weight is added, insulated and stirred 10-20 minutes, obtains amination monomeric polyol liquid；
(9) ammonium persulfate for taking 3-4 parts by weight is added in the deionized water of 60-70 times of its weight, stirs evenly, obtains over cure
Sour aqueous ammonium；
(10) the hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, is stirred evenly, is sent to anti-
It answers in kettle, the stannous octoate of 1-3 parts by weight is added, insulated and stirred 20-30 minutes at 40-50 DEG C, be passed through nitrogen, be added above-mentioned
Ammonium persulfate aqueous solution stirs evenly, and adjusting temperature of reaction kettle is 68-71 DEG C, and insulation reaction 4-5 hours, 13-20 weight is added
Part pentane foaming agent, increase temperature be 110-120 DEG C, keep the temperature 1-2 hour, cooling discharging, by product by washing, drying,
It being sent in foaming machine after screening, steam heats 1-2 hours at 0.25-0.3MPa, 130-140 DEG C, and discharging, room temperature is cooling,
Up to the sol deposition hollow polystyrene building thermal insulation material.
2. a kind of preparation method of sol deposition hollow polystyrene building thermal insulation material according to claim 1, special
Sign is that the initiator is one of azodiisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide.
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| CN101289519A (en) * | 2008-06-10 | 2008-10-22 | 上海碧虎节能保温材料有限公司 | Preparation of organic-inorganic composite foam material |
| CN103627073A (en) * | 2013-10-23 | 2014-03-12 | 吴学三 | Polyethylene-polystyrene foam |
| CN104058630B (en) * | 2014-04-24 | 2016-05-18 | 青岛伟源达技术服务有限公司 | A kind of novel heat insulation plate and preparation method thereof |
| CN105294041A (en) * | 2015-11-06 | 2016-02-03 | 合肥神舟建筑集团有限公司 | Homogeneous modified fireproof heat insulation board |
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2017
- 2017-04-14 CN CN201710246027.2A patent/CN106977829B/en active Active
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