CN105967550A - Anti-aging expanded perlite and phenolic resin composite insulation board and preparation method thereof - Google Patents

Anti-aging expanded perlite and phenolic resin composite insulation board and preparation method thereof Download PDF

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Publication number
CN105967550A
CN105967550A CN201610178170.8A CN201610178170A CN105967550A CN 105967550 A CN105967550 A CN 105967550A CN 201610178170 A CN201610178170 A CN 201610178170A CN 105967550 A CN105967550 A CN 105967550A
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China
Prior art keywords
expanded perlite
parts
phenolic resin
silicon
stirring
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CN201610178170.8A
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Chinese (zh)
Inventor
董良清
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Dangtu County Kehui Trading Co Ltd
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Dangtu County Kehui Trading Co Ltd
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Priority to CN201610178170.8A priority Critical patent/CN105967550A/en
Publication of CN105967550A publication Critical patent/CN105967550A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/10Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/12Condensation polymers of aldehydes or ketones
    • C04B26/122Phenol-formaldehyde condensation polymers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/04Silica-rich materials; Silicates
    • C04B14/14Minerals of vulcanic origin
    • C04B14/18Perlite
    • C04B14/185Perlite expanded
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00008Obtaining or using nanotechnology related materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Building Environments (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention discloses an anti-aging expanded perlite and phenolic resin composite insulation board, which is prepared from the following raw materials (by weight): 0.8-1 part of methyl methacrylate, 2-2.4 parts of silicon-aluminum sol, 6-7 parts of hydroxyapatite, 1.3-1.6 parts of silicon tetrachloride, 55-57 parts of expanded perlite, 40-42 parts of phenolic resin, 4-4.1 parts of a curing agent HMTA, 2-2.3 parts of steel fiber, 10-11 parts of tetraethyl orthosilicate, a proper amount of 85wt% ammonia water, a proper amount of anhydrous ethanol, 160-180 parts of deionized water, a proper amount of n-hexane, 4-4.5 parts of nano-polytetrafluoroethylene, 0.1-0.2 part of dicumyl peroxide and 3-3.5 parts of 2,2,2-trifluoroethyl acrylate. By using methyl methacrylate and silicon tetrachloride for modification of hydroxyapatite, compatibility of hydroxyapatite and resin is raised, and aging resistance and heat resistance of the insulation board can be boosted. By the use of silicon-aluminum sol, heat insulating property and aging resistance of the insulation board are improved.

Description

A kind of aging resistance expanded perlite phenolic resin composite insulation boards and preparation method thereof
Technical field
The present invention relates to heat-insulation wall plate technical field, particularly relate to a kind of aging resistance expanded perlite phenolic resin composite insulation boards and preparation method thereof.
Background technology
Compound insulating material (CompositeInsulationMaterials) is to be combined homogeneous new material by two or more insulation material, be often referred to the compound of organic insulation material and inorganic heat insulation material, compound after the performance of more original machine or inorganic material more excellent.Make full use of the perlite Advantage of Mineral Resources that Xinyang is abundant herein, with expanded perlite (ExpendedPerlite, and phenolic resin (Phenol-formaldchydeResin EP), PF) it is primary raw material, add the auxiliary agents such as appropriate firming agent, toughener and hydrophober, the most hot-forming, it is prepared as expanded perlite/phenolic resin compound insulating material.Paper main research includes: the proportioning of (1) primary raw material and the optimization of compression ratio;(2) under conditions of phenolic resin consumption and compression ratio are certain, use the factor impacts on compound insulating material performance such as the hot-forming temperature of monofactorial Research on experimental methods, dwell time and hardener dose, thus primarily determine that the parameter index of each influence factor;(3) on experiment of single factor Research foundation, use orthogonal experiment, optimization Test condition, selection optimal parameter combines, and inquired into the reciprocal action between the factors such as hot-forming temperature, dwell time and hardener dose, use directly perceived analysis and variance analysis, experiment condition is investigated.Result proves, hot-forming temperature and hardener dose are the notable factors affecting compound insulating material performance;(4) to the physical property of material [apparent density, heat conductivity, water absorption rate), mechanical property (rupture strength, comprcssive strength, elastic modelling quantity, shock resistance) and microstructure test and characterize;(5) on the Research foundation of orthogonal test, adding suitable toughener and hydrophober, toughness and water absorption rate to compound insulating material are optimized.Test result indicate that, preferably preparation condition is: compression ratio, 2.0;Phenolic resin consumption, 40%;Hot-forming temperature, 240 DEG C;Dwell time, 1.5h;Firming agent (HMTA) consumption, 4%;Toughener (fiber) volume, 2%;Hydrophober (BS1042) volume, 0.6%.Under the conditions of more excellent, the apparent density of compound insulating material is 332.4kg/m3, heat conductivity is 0.047W/ (m K), and rupture strength is 1.436MPa, and comprcssive strength is 1.652MPa, and elastic modelling quantity is 2.496MPa, and impact strength is 147.26kJ/m2, water absorption rate is 2.03%.Compound insulating material prepared by this problem overcomes the deficiency that inorganic heat insulation material heat conductivity is bigger than normal, compensate for the shortcomings such as organic insulation material fire protection flame retarding and loss of properties on aging, has actual application value.
But expanded perlite water absorption rate is high, poor water resistance causes thermal insulation mortar volume contraction deformation in stirring big, and product later stage heat-insulating property reduces low with bond matrix intensity, affect later stage wallboard heat-insulating property.
It is thus desirable to composite is further improved, meet the needs of heat-insulation wall plate development, need to improve the performances such as the resistance to water of warming plate, heat insulating ability, thermostability, anti-flammability, durability, toughness, resilience, crushing resistance, sound-proofing, bend resistance, aging resistance, radioprotective, protection against the tide.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of aging resistance expanded perlite phenolic resin composite insulation boards and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of aging resistance expanded perlite phenolic resin composite insulation boards, is prepared by the raw materials in: methyl methacrylate 0.8-1, silicon-aluminum sol 2-2.4, hydroxyapatite 6-7, Silicon chloride. 1.3-1.6, expanded perlite 55-57, phenolic resin 40-42, firming agent HMTA4-4.1, steel fibre 2-2.3, tetraethyl orthosilicate 10-11,85wt% ammonia are appropriate, dehydrated alcohol appropriate, deionized water 160-180, normal hexane are appropriate, nanometer polytetrafluoroethylcomposite 4-4.5, dicumyl peroxide 0.1-0.2, acrylic acid trifluoro ethyl ester 3-3.5.
The preparation method of described aging resistance expanded perlite phenolic resin composite insulation boards, comprises the following steps:
(1) hydroxyapatite is pulverized, cross 300 mesh sieves, then mix with the dehydrated alcohol of 3-4 times of weight portion, stir, it is heated to 85-90 DEG C, insulated and stirred 20-30 minute, add methyl methacrylate, Silicon chloride., stir, continuing insulated and stirred until being dried, obtaining powder;
(2) expanded perlite is mixed with dehydrated alcohol, the deionized water of 55-60 weight portion, it is heated with stirring to 44-47 DEG C in a water bath, adding 85wt% ammonia regulation pH is 8-9, tetraethyl orthosilicate is dripped after continuing stirring 10-12min, constant temperature 44-47 DEG C stirring reaction 4-4.3h after dropping, reaction is cooled to room temperature after stopping and obtaining mixed material;
(3) mixed material that the powder (1st) step obtained and (2nd) step obtain adds the ethanol of 2-2.5 times of volume and stirs, ageing 48h, it is filtrated to get filtrate, again filtrate is immersed in the normal hexane of 2-2.5 times of volume, filter, by filtrate freeze-day with constant temperature at 45-46 DEG C, obtain modified expanded perlite;
(4) nanometer polytetrafluoroethylcomposite, acrylic acid trifluoro ethyl ester, silicon-aluminum sol are mixed with the dehydrated alcohol of 20-25 weight portion, it is heated to 60-70 DEG C, add dicumyl peroxide, stirring reaction 30-40 minute, obtaining glue, the stirring of modified expanded perlite limit seethed, the most described glue is sprayed on limit, continuing stirring after sprayed to seethe until being dried, obtaining powder;
(5) powder that (4th) step obtains is mixed homogeneously with other residual componentss, extruded in vacuum environment, it is again heated to 240-245 DEG C, compression ratio is 1.8-2.0, suppresses 1.5-1.6h, to obtain final product.
The invention have the advantage that the present invention uses tetraethyl orthosilicate to be modified expanded perlite, expanded perlite pore interior is made to have nano level hole, improve heat insulation effect, and the coarse thin film with activity hydroxy is defined on the surface of expanded perlite, improve expanded perlite and the compatibility of phenolic resin and adhesion, improve the intensity of warming plate;By using nanometer polytetrafluoroethylcomposite, acrylic acid trifluoro ethyl ester to be coated with perlite surface, preventing perlite water suction from causing nanoaperture to be destroyed, heat-insulating property declines, and extends service life;By using methyl methacrylate, Silicon chloride. that hydroxyapatite is modified, improve the compatibility of hydroxyapatite and resin, it is possible to increase the ageing resistance of warming plate and thermostability;By using silicon-aluminum sol, it is possible to increase the resistance to water of expanded perlite, thus improve heat insulating ability and the resistance to ag(e)ing of warming plate.
Detailed description of the invention
A kind of aging resistance expanded perlite phenolic resin composite insulation boards, is made up of the raw material of following weight portion (kilogram): methyl methacrylate 0.8, silicon-aluminum sol 2, hydroxyapatite 6, Silicon chloride. 1.3, expanded perlite 55, phenolic resin 40, firming agent HMTA4, steel fibre 2, tetraethyl orthosilicate 10,85wt% ammonia are appropriate, dehydrated alcohol appropriate, deionized water 160, normal hexane are appropriate, nanometer polytetrafluoroethylcomposite 4, dicumyl peroxide 0.1, acrylic acid trifluoro ethyl ester 3.
The preparation method of described aging resistance expanded perlite phenolic resin composite insulation boards, comprises the following steps:
(1) hydroxyapatite is pulverized, cross 300 mesh sieves, then mix with the dehydrated alcohol of 3 times of weight portions, stir, it is heated to 85 DEG C, insulated and stirred 20 minutes, add methyl methacrylate, Silicon chloride., stir, continuing insulated and stirred until being dried, obtaining powder;
(2) by expanded perlite and the dehydrated alcohol of 55 weight portions, deionized water mixing, it is heated with stirring to 44 DEG C in a water bath, adding 85wt% ammonia regulation pH is 8, tetraethyl orthosilicate is dripped after continuing stirring 10min, constant temperature 44 DEG C stirring reaction 4h after dropping, reaction is cooled to room temperature after stopping and obtaining mixed material;
(3) mixed material that the powder (1st) step obtained and (2nd) step obtain adds the ethanol of 2 times of volumes and stirs, and is aged 48h, is filtrated to get filtrate, again filtrate is immersed in the normal hexane of 2 times of volumes, filter, by filtrate freeze-day with constant temperature at 45 DEG C, obtain modified expanded perlite;
(4) dehydrated alcohol of nanometer polytetrafluoroethylcomposite, acrylic acid trifluoro ethyl ester, silicon-aluminum sol and 20 weight portions is mixed, it is heated to 60 DEG C, add dicumyl peroxide, stirring reaction 30 minutes, obtaining glue, the stirring of modified expanded perlite limit seethed, the most described glue is sprayed on limit, continuing stirring after sprayed to seethe until being dried, obtaining powder;
(5) powder that (4th) step obtains is mixed homogeneously with other residual componentss, extruded in vacuum environment, it is again heated to 240 DEG C, compression ratio is 1.8, suppresses 1.5h, to obtain final product.
The apparent density of the warming plate of this embodiment is 309.4kg/m3, heat conductivity is 0.025W/ (m K), and rupture strength is 1.623MPa, and comprcssive strength is 1.732MPa, and elastic modelling quantity is 2.68MPa, and impact strength is 155kJ/m2, water absorption rate is 1.08%.

Claims (2)

1. an aging resistance expanded perlite phenolic resin composite insulation boards, it is characterised in that: it is prepared by the raw materials in: methyl methacrylate 0.8-1, silicon-aluminum sol 2-2.4, hydroxyapatite 6-7, Silicon chloride. 1.3-1.6, expanded perlite 55-57, phenolic resin 40-42, firming agent HMTA4-4.1, steel fibre 2-2.3, tetraethyl orthosilicate 10-11,85wt% ammonia are appropriate, dehydrated alcohol appropriate, deionized water 160-180, normal hexane are appropriate, nanometer polytetrafluoroethylcomposite 4-4.5, dicumyl peroxide 0.1-0.2, acrylic acid trifluoro ethyl ester 3-3.5.
The preparation method of aging resistance expanded perlite phenolic resin composite insulation boards the most according to claim 1, it is characterised in that comprise the following steps:
(1) hydroxyapatite is pulverized, cross 300 mesh sieves, then mix with the dehydrated alcohol of 3-4 times of weight portion, stir, it is heated to 85-90 DEG C, insulated and stirred 20-30 minute, add methyl methacrylate, Silicon chloride., stir, continuing insulated and stirred until being dried, obtaining powder;
(2) expanded perlite is mixed with dehydrated alcohol, the deionized water of 55-60 weight portion, it is heated with stirring to 44-47 DEG C in a water bath, adding 85wt% ammonia regulation pH is 8-9, tetraethyl orthosilicate is dripped after continuing stirring 10-12min, constant temperature 44-47 DEG C stirring reaction 4-4.3h after dropping, reaction is cooled to room temperature after stopping and obtaining mixed material;
(3) mixed material that the powder (1st) step obtained and (2nd) step obtain adds the ethanol of 2-2.5 times of volume and stirs, ageing 48h, it is filtrated to get filtrate, again filtrate is immersed in the normal hexane of 2-2.5 times of volume, filter, by filtrate freeze-day with constant temperature at 45-46 DEG C, obtain modified expanded perlite;
(4) nanometer polytetrafluoroethylcomposite, acrylic acid trifluoro ethyl ester, silicon-aluminum sol are mixed with the dehydrated alcohol of 20-25 weight portion, it is heated to 60-70 DEG C, add dicumyl peroxide, stirring reaction 30-40 minute, obtaining glue, the stirring of modified expanded perlite limit seethed, the most described glue is sprayed on limit, continuing stirring after sprayed to seethe until being dried, obtaining powder;
(5) powder that (4th) step obtains is mixed homogeneously with other residual componentss, extruded in vacuum environment, it is again heated to 240-245 DEG C, compression ratio is 1.8-2.0, suppresses 1.5-1.6h, to obtain final product.
CN201610178170.8A 2016-03-28 2016-03-28 Anti-aging expanded perlite and phenolic resin composite insulation board and preparation method thereof Withdrawn CN105967550A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10336941B2 (en) 2017-06-13 2019-07-02 International Business Machines Corporation Impact-modified hydroxyapatite as flame retardant polymer fillers
CN110295677A (en) * 2019-05-22 2019-10-01 同济大学 Integrated super-hydrophobic particle and its preparation method and application is insulated for assembled architecture seam waterproof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102787670A (en) * 2012-07-06 2012-11-21 万国骅 Fire-proof and thermal-insulation board and manufacturing method thereof
CN104058630A (en) * 2014-04-24 2014-09-24 潍坊纳博欧化工科技有限公司 Novel heat insulating plate and manufacturing method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102787670A (en) * 2012-07-06 2012-11-21 万国骅 Fire-proof and thermal-insulation board and manufacturing method thereof
CN104058630A (en) * 2014-04-24 2014-09-24 潍坊纳博欧化工科技有限公司 Novel heat insulating plate and manufacturing method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10336941B2 (en) 2017-06-13 2019-07-02 International Business Machines Corporation Impact-modified hydroxyapatite as flame retardant polymer fillers
US10570336B2 (en) 2017-06-13 2020-02-25 International Business Machines Corporation Impact-modified hydroxyapatite as flame retardant polymer fillers
CN110295677A (en) * 2019-05-22 2019-10-01 同济大学 Integrated super-hydrophobic particle and its preparation method and application is insulated for assembled architecture seam waterproof

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