CN106977829A - 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 PDF

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CN106977829A
CN106977829A CN201710246027.2A CN201710246027A CN106977829A CN 106977829 A CN106977829 A CN 106977829A CN 201710246027 A CN201710246027 A CN 201710246027A CN 106977829 A CN106977829 A CN 106977829A
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赵阳
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Nanjing AAA Energy Saving Materials Co Ltd
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L25/00Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
    • C08L25/02Homopolymers or copolymers of hydrocarbons
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    • C08F112/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F112/02Monomers containing only one unsaturated aliphatic radical
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12Working-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
    • C08J9/14Working-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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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
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    • C08K9/00Use of pretreated ingredients
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    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
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    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/14Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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    • C08J2325/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02Homopolymers or copolymers of hydrocarbons
    • C08J2325/04Homopolymers or copolymers of styrene
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract

The invention discloses a kind of preparation method 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, in the polymerisation for participating in styrene, effectively raise compatibility of the filler between polymer, reunion is effectively reduced, the stability_intensity of finished-product material is improved.The composite of the present invention has good fire-retardant, insulation, anti-corrosion, stability_intensity etc., and light weight, and the feature of environmental protection is good, and combination property is superior.

Description

A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation of sol deposition hollow polystyrene building thermal insulation material Method.
Background technology
Polystyrene foamed material is, using polystyrene resin as base-material, to add the auxiliary materials, heated hair such as foaming agent The light material of bubble.It has that light weight, thermal conductivity factor are small, water absorption rate is low, water-fast, ageing-resistant, low temperature resistant, easy processing, valency Honest and clean of fine quality the advantages of, but polystyrene foam heat insulation material is while the life given people brings huge facilitate, its is inflammable Property also brings certain limitation to its application.Polystyrene foam is combustible material in itself, under fire and hot conditions Easily decompose burning,
And produced with a large amount of poison gases.Therefore, it is badly in need of carrying out to grinding in terms of polystyrene foam heat insulation material fire safety Study carefully work;
The purposes of foamed polystyrene resin widely, because it has high intensity, light weight, splendid insulation heat-insulating property With high-selenium corn energy ability, the packaging of various instrument, valuables, precision instrument, vegetable and fruit and aquatic products etc. may be used as Material;And because its have that pyroconductivity is low, water imbibition is small, electrical insulating property good, sound insulation, protection against the tide and moulding process it is simply etc. excellent Good characteristic, and the insulation of industry is fished for and refrigerated in the roadbed laying and building construction and fishery for being widely used in road and bridge In terms of material.Wherein, as a kind of excellent construction material, foamed polystyrene resin be mainly used in building roofing and Wall, it has very good energy-saving effect as external heat insulating composite wall;And it is applied to house, work as heat insulation house surface Factory, flat and pitch roofing, can play the effect such as sound insulation, dash steam, sealing and insulation.It is used as thermal insulating material for building Material, several performance indications of overriding concern are low thermal conductivities, high fire retardancy, preferable self-strength;
At present, in order to improve the performances such as the fire-retardant of insulation material, self-strength, insulation, it will usually introduce inorganic filler, but nothing The compatibility of machine filler and polymeric matrix is poor, is easily caused the stability reduction of finished product, and is passed through in Conventional insulation Hollow glass micropearl can be often added, it has the heat-insulating property for improving material well, but its cost is higher, and fragile Split.
The content of the invention
It is an object of the invention to the compatibility for inorganic filler in the prior art and polymeric matrix is poor, cost compared with High the problem of, there is provided a kind of preparation method of sol deposition hollow polystyrene building thermal insulation material.
To achieve the above object, the present invention uses following technical scheme:
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, comprises the following steps:
(1)Terephthalaldehyde, the methyl methacrylate mixing of 20-27 parts by weight of 1-2 parts by weight are taken, stirs, adds Compound weight 30-40% methanol, is stirred, is sent in reactor, be passed through nitrogen, and 40-50 is incubated at 60-70 DEG C Minute, obtain aldehyde radical monomer;
(2)Above-mentioned aldehyde radical monomer, the initiator mixing of 0.2-0.4 parts by weight are taken, the tetrahydrochysene of 6-9 times of compound weight is added to In furans, it is sent in reactor, insulation reaction 6-7 hours at 80-85 DEG C, discharging is cooled to normal temperature, 45-50 DEG C of vacuum Lower dry 2-3 hours, obtain aldehyde radical fluidized polymer;
(3)The tetraethyl orthosilicate of 17-20 parts by weight is taken, in the deionized water for being added to 30-40 times of its weight, 16-20 points of stirring Clock, obtains precursor solution;
(4)The calcium carbonate of 20-30 parts by weight is taken, in the absolute ethyl alcohol for being added to 3-4 times of its weight, is stirred, 2-4 weights are added The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 20-30 minutes, are distilled off ethanol 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, is added in above-mentioned precursor solution, be added dropwise The 10-13% of 3-5 parts by weight ammoniacal liquor, rise temperature is 50-60 DEG C, and insulated and stirred 2-3 hours turns at 2700-3000 revs/min Speed is lower to be centrifuged, and precipitation is washed, is dried 30-40 minutes 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, 46-50 DEG C of thermostatted water is sent to In bath, 10-13 hours are incubated, is discharged, filtering washs precipitation 2-3 times with acetone, deionized water, air drying, in obtaining successively Empty sol deposition pearl filler;
(7)Take in above-mentioned hollow sol deposition pearl filler, the absolute ethyl alcohol for being added to 1.5-2 times of its weight, add 2-3 weights The epoxychloropropane of part is measured, it is ultrasonic 10-20 minutes, ethanol is distilled off, the hollow sol deposition pearl filler of epoxidation is obtained;
(8)The lauryl amine of 4-5 parts by weight is taken, in the absolute ethyl alcohol for being added to 3-5 times of its weight, is stirred, rise temperature 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)The ammonium persulfate of 3-4 parts by weight is taken, in the deionized water for being added to 60-70 times of its weight, is stirred;
(10)The hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, stirred, is sent to anti- Answer in kettle, add the stannous octoate of 1-3 parts by weight, insulated and stirred 20-30 minutes at 40-50 DEG C, be passed through nitrogen, add above-mentioned Ammonium persulfate aqueous solution, stirs, and regulation temperature of reaction kettle is 68-71 DEG C, and insulation reaction 4-5 hours adds 13-20 weight Part pentane foaming agent, rise temperature is 110-120 DEG C, is incubated 1-2 hour, cooling discharging, by product by washing, it is dry, It is sent to after screening in foaming machine, steam is heated 1-2 hours at 0.25-0.3Mpa, 130-140 DEG C, discharging, room temperature cooling, Produce the sol deposition hollow polystyrene building thermal insulation material.
Described initiator is one kind in azodiisobutyronitrile, ABVN, benzoyl peroxide.
Advantages of the present invention:
The present invention is mixed using terephthalaldehyde, methyl methacrylate first, obtains aldehyde radical monomer, then this monomer exists It is polymerize under the conditions of initiator, obtains aldehyde radical fluidized polymer, then carry out blended cross linking with ammonification calcium carbonate, while crosslinking It is scattered by high speed centrifugation in being added to using tetraethyl orthosilicate as the sol solutionses of presoma so that Ludox deposits to crosslinking production The surface of thing, forms the clad of Ludox, and be crosslinked obtained schiff bases has good stability in the basic conditions, and The antibacterial antiseptic property of finished product can be improved, sol deposition polymer is added in acetone afterwards, makes poly-methyl methacrylate Ester dissolving is removed, and is obtained the hollow pearl filler of Sol-gel Coated, is then passed through the hollow pearl filler of the Sol-gel Coated Epoxidation processing, is blended with amination styrene monomer, in the polymerisation for participating in styrene monomer, then by foaming, obtains Sol deposition hollow polystyrene building thermal insulation material;
The insulation material of the present invention contains the hollow pearl filler of Sol-gel Coated, the filler light weight, due to there is the bag of Ludox Protection is covered, is not easily broken, stability is good, being incubated of finished-product material, fire-retardant, mechanical property can be not only improved, also reduce into The weight of product, has reached the effect of lightweight, is readily transported, installs, and reduces production cost, and its cost is relative to hollow glass Microballon is relatively low, can further reduce production cost;
The present invention will be blended after hollow sol deposition pearl filler epoxidation with amination styrene monomer, participate in styrene In polymerisation, compatibility of the filler between polymer is effectively raised, reunion is effectively reduced, improves finished-product material Stability_intensity.
The composite of the present invention has good fire-retardant, insulation, anti-corrosion, stability_intensity etc., and light weight, the feature of environmental protection Good, combination property is superior.
Embodiment
Embodiment 1
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, comprises the following steps:
(1)Terephthalaldehyde, the methyl methacrylate mixing of 27 parts by weight of 2 parts by weight are taken, stirs, adds compound The methanol of weight 40%, stirs, and is sent in reactor, is passed through nitrogen, is incubated 50 minutes at 70 DEG C, obtains aldehyde radical list Body;
(2)Above-mentioned aldehyde radical monomer, the ABVN mixing of 0.4 parts by weight are taken, the tetrahydrochysene of 9 times of compound weight is added to In furans, it is sent in reactor, insulation reaction 7 hours at 85 DEG C, discharges, is cooled at normal temperature, 50 DEG C of vacuum dry 3 small When, obtain aldehyde radical fluidized polymer;
(3)The tetraethyl orthosilicate of 20 parts by weight is taken, in the deionized water for being added to 40 times of its weight, stirs 20 minutes, obtains forerunner Liquid solution;
(4)The calcium carbonate of 30 parts by weight is taken, in the absolute ethyl alcohol for being added to 4 times of its weight, is stirred, 4 parts by weight are added Gamma-aminopropyl-triethoxy-silane, ultrasound 30 minutes, are distilled off ethanol, obtain ammonification calcium carbonate at 60 DEG C;
(5)Above-mentioned aldehyde radical fluidized polymer, the mixing of ammonification calcium carbonate are taken, stirs, is added in above-mentioned precursor solution, be added dropwise The 10-13% of 5 parts by weight ammoniacal liquor, rise temperature is 60 DEG C, and insulated and stirred 3 hours is centrifuged under 3000 revs/min of rotating speeds, Precipitation is washed, is dried 40 minutes at 80 DEG C of vacuum, obtains sol deposition polymer;
(6)In the acetone that above-mentioned sol deposition polymer is added to 13 times of its weight, in the water bath with thermostatic control for being sent to 50 DEG C, protect Temperature 13 hours, is discharged, and precipitation is washed 2 times, air drying, obtains hollow sol deposition carbon by filtering successively with acetone, deionized water Sour calcium filler;
(7)Take in above-mentioned hollow sol deposition pearl filler, the absolute ethyl alcohol for being added to 2 times of its weight, add 2 parts by weight Epoxychloropropane, ultrasound 20 minutes, is distilled off ethanol, obtains the hollow sol deposition pearl filler of epoxidation;
(8)The lauryl amine of 5 parts by weight is taken, in the absolute ethyl alcohol for being added to 5 times of its weight, is stirred, rise temperature is 60 DEG C, The styrene of 200 parts by weight is added, insulated and stirred 20 minutes obtains amination monomeric polyol liquid;
(9)The ammonium persulfate of 4 parts by weight is taken, in the deionized water for being added to 70 times of its weight, is stirred;
(10)The hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, stirred, is sent to anti- Answer in kettle, add the stannous octoate of 3 parts by weight, insulated and stirred 30 minutes at 50 DEG C are passed through nitrogen, add above-mentioned ammonium persulfate The aqueous solution, stirs, and regulation temperature of reaction kettle is 68-71 DEG C, and insulation reaction 5 hours adds the pentane-blown of 20 parts by weight Agent, rise temperature is 120 DEG C, is incubated 2 hours, cooling discharging, and product is sent into foaming machine after washing, dry, screening In, steam is heated 2 hours at 0.3Mpa, 140 DEG C, discharging, room temperature cooling, is produced the sol deposition hollow polystyrene and is built Building thermal insulation material.
Performance test:
The fire resistance of the sol deposition hollow polystyrene building thermal insulation material of the present embodiment 1, mechanical experimental results table It is bright:
Oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, bending strength 0.27Mpa, compressive strength 0.21Mpa, heat conduction Coefficient 0.029w/m.k.
Embodiment 2
A kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, comprises the following steps:
(1)Terephthalaldehyde, the methyl methacrylate mixing of 20 parts by weight of 1 parts by weight are taken, stirs, adds compound The methanol of weight 30%, stirs, and is sent in reactor, is passed through nitrogen, is incubated 40 minutes at 60 DEG C, obtains aldehyde radical list Body;
(2)Above-mentioned aldehyde radical monomer, the azodiisobutyronitrile mixing of 0.2 parts by weight are taken, the tetrahydrochysene of 6 times of compound weight is added to In furans, it is sent in reactor, insulation reaction 6 hours at 80 DEG C, discharges, is cooled at normal temperature, 45 DEG C of vacuum dry 2 small When, obtain aldehyde radical fluidized polymer;
(3)The tetraethyl orthosilicate of 17 parts by weight is taken, in the deionized water for being added to 30 times of its weight, stirs 16 minutes, obtains forerunner Liquid solution;
(4)The calcium carbonate of 20 parts by weight is taken, in the absolute ethyl alcohol for being added to 3 times of its weight, is stirred, 4 parts by weight are added Gamma-aminopropyl-triethoxy-silane, ultrasound 20 minutes, are distilled off ethanol, obtain ammonification calcium carbonate at 50 DEG C;
(5)Above-mentioned aldehyde radical fluidized polymer, the mixing of ammonification calcium carbonate are taken, stirs, is added in above-mentioned precursor solution, be added dropwise 10% ammoniacal liquor of 3 parts by weight, rise temperature is 50 DEG C, and insulated and stirred 2 hours is centrifuged under 2700 revs/min of rotating speeds, will Dried 30 minutes at precipitation washing, 70 DEG C of vacuum, obtain sol deposition polymer;
(6)In the acetone that above-mentioned sol deposition polymer is added to 10 times of its weight, in the water bath with thermostatic control for being sent to 46 DEG C, protect Temperature 10 hours, is discharged, and precipitation is washed 2 times, air drying, obtains hollow sol deposition carbon by filtering successively with acetone, deionized water Sour calcium filler;
(7)Take in above-mentioned hollow sol deposition pearl filler, the absolute ethyl alcohol for being added to 1.5 times of its weight, add 2 parts by weight Epoxychloropropane, ultrasound 10 minutes, ethanol is distilled off, the hollow sol deposition pearl filler of epoxidation is obtained;
(8)The lauryl amine of 4 parts by weight is taken, in the absolute ethyl alcohol for being added to 3 times of its weight, is stirred, rise temperature is 50 DEG C, The styrene of 190 parts by weight is added, insulated and stirred 10 minutes obtains amination monomeric polyol liquid;
(9)The ammonium persulfate of 3 parts by weight is taken, in the deionized water for being added to 60 times of its weight, is stirred;
(10)The hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, stirred, is sent to anti- Answer in kettle, add the stannous octoate of 1 parts by weight, insulated and stirred 20 minutes at 40 DEG C are passed through nitrogen, add above-mentioned ammonium persulfate The aqueous solution, stirs, and regulation temperature of reaction kettle is 68 DEG C, and insulation reaction 4 hours adds the pentane foaming agent of 13 parts by weight, It is 110 DEG C to raise temperature, is incubated 1 hour, cooling discharging, and product is sent in foaming machine after washing, dry, screening, Steam is heated 1 hour at 0.25Mpa, 130 DEG C, discharging, room temperature cooling, produces the sol deposition hollow polystyrene building Insulation material.
Performance test:
The fire resistance of the sol deposition hollow polystyrene building thermal insulation material of the present embodiment 2, mechanical experimental results table It is bright:
Oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, bending strength 0.26Mpa, compressive strength 0.20Mpa, heat conduction Coefficient 0.029w/m.k.

Claims (2)

1. a kind of preparation method of sol deposition hollow polystyrene building thermal insulation material, it is characterised in that comprise the following steps:
(1)Terephthalaldehyde, the methyl methacrylate mixing of 20-27 parts by weight of 1-2 parts by weight are taken, stirs, adds Compound weight 30-40% methanol, is stirred, is sent in reactor, be passed through nitrogen, and 40-50 is incubated at 60-70 DEG C Minute, obtain aldehyde radical monomer;
(2)Above-mentioned aldehyde radical monomer, the initiator mixing of 0.2-0.4 parts by weight are taken, the tetrahydrochysene of 6-9 times of compound weight is added to In furans, it is sent in reactor, insulation reaction 6-7 hours at 80-85 DEG C, discharging is cooled to normal temperature, 45-50 DEG C of vacuum Lower dry 2-3 hours, obtain aldehyde radical fluidized polymer;
(3)The tetraethyl orthosilicate of 17-20 parts by weight is taken, in the deionized water for being added to 30-40 times of its weight, 16-20 points of stirring Clock, obtains precursor solution;
(4)The calcium carbonate of 20-30 parts by weight is taken, in the absolute ethyl alcohol for being added to 3-4 times of its weight, is stirred, 2-4 weights are added The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 20-30 minutes, are distilled off ethanol 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, is added in above-mentioned precursor solution, be added dropwise The 10-13% of 3-5 parts by weight ammoniacal liquor, rise temperature is 50-60 DEG C, and insulated and stirred 2-3 hours turns at 2700-3000 revs/min Speed is lower to be centrifuged, and precipitation is washed, is dried 30-40 minutes 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, 46-50 DEG C of thermostatted water is sent to In bath, 10-13 hours are incubated, is discharged, filtering washs precipitation 2-3 times with acetone, deionized water, air drying, in obtaining successively Empty sol deposition pearl filler;
(7)Take in above-mentioned hollow sol deposition pearl filler, the absolute ethyl alcohol for being added to 1.5-2 times of its weight, add 2-3 weights The epoxychloropropane of part is measured, it is ultrasonic 10-20 minutes, ethanol is distilled off, the hollow sol deposition pearl filler of epoxidation is obtained;
(8)The lauryl amine of 4-5 parts by weight is taken, in the absolute ethyl alcohol for being added to 3-5 times of its weight, is stirred, rise temperature 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)The ammonium persulfate of 3-4 parts by weight is taken, in the deionized water for being added to 60-70 times of its weight, is stirred;
(10)The hollow sol deposition pearl filler of above-mentioned epoxidation, amination monomeric polyol liquid are mixed, stirred, is sent to anti- Answer in kettle, add the stannous octoate of 1-3 parts by weight, insulated and stirred 20-30 minutes at 40-50 DEG C, be passed through nitrogen, add above-mentioned Ammonium persulfate aqueous solution, stirs, and regulation temperature of reaction kettle is 68-71 DEG C, and insulation reaction 4-5 hours adds 13-20 weight Part pentane foaming agent, rise temperature is 110-120 DEG C, is incubated 1-2 hour, cooling discharging, by product by washing, it is dry, It is sent to after screening in foaming machine, steam is heated 1-2 hours at 0.25-0.3Mpa, 130-140 DEG C, discharging, room temperature cooling, Produce 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, it is special Levy and be, described initiator is one kind in azodiisobutyronitrile, ABVN, benzoyl peroxide.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107236277A (en) * 2017-07-26 2017-10-10 汪青霞 A kind of preparation method of hollow insulation polyester material
CN107556444A (en) * 2017-08-23 2018-01-09 安徽富煌门窗幕墙有限公司 One kind coats sol-gel modified building heat preservation sheet material and preparation method thereof
CN109354636A (en) * 2018-09-20 2019-02-19 刘彦彦 A kind of light-weight environment-friendly polystyrol foam material and preparation method thereof

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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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CN103627073A (en) * 2013-10-23 2014-03-12 吴学三 Polyethylene-polystyrene foam
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* Cited by examiner, † Cited by third party
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CN107236277A (en) * 2017-07-26 2017-10-10 汪青霞 A kind of preparation method of hollow insulation polyester material
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CN109354636A (en) * 2018-09-20 2019-02-19 刘彦彦 A kind of light-weight environment-friendly polystyrol foam material and preparation method thereof

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