CN102701687A - Insulated fireproof material of polyurethane cement foam and preparation method of insulated fireproof material - Google Patents

Insulated fireproof material of polyurethane cement foam and preparation method of insulated fireproof material Download PDF

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Publication number
CN102701687A
CN102701687A CN2012102196277A CN201210219627A CN102701687A CN 102701687 A CN102701687 A CN 102701687A CN 2012102196277 A CN2012102196277 A CN 2012102196277A CN 201210219627 A CN201210219627 A CN 201210219627A CN 102701687 A CN102701687 A CN 102701687A
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China
Prior art keywords
cement
polyurethane
retardant
thermal insulation
parts
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Pending
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CN2012102196277A
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Chinese (zh)
Inventor
胡先海
罗俊杰
罗志勇
付昌春
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ANHUI SIWEI NEW BUILDING MATERIAL Co Ltd
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ANHUI SIWEI NEW BUILDING MATERIAL Co Ltd
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Priority to CN2012102196277A priority Critical patent/CN102701687A/en
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Abstract

The invention discloses an insulated fireproof material of polyurethane cement foam and a preparation method of the insulated fireproof material. The insulated fireproof material comprises 50-70 parts of cement, 27-32 parts of water, 1.5-2 parts of foaming agent, 0.2-0.5 parts of early strength agent, 0.5-1.5 parts of water reducer and 5-25 parts of soluble polyurethane. The insulated fireproof material of polyurethane cement foam disclosed by the invention is prepared by the processes of leading in a lot of miniature, stable and sealed air bubbles and a little of polyurethane into cement, and uniformly dispersing the air bubbles and polyurethane in cement matrix. The insulated fireproof material overcomes the defects that inorganic material is easy to pulverize, low in strength and poor in heat preservation effect, and has the advantages of light material, sound insulation, thermostability, large elasticity modulus, corrosion resistance, durability and the like.

Description

A kind of polyurethane cement foam thermal insulation fire-retardant material and preparation method thereof
Technical field
What the present invention relates to is a kind of material of construction with fireproof heat insulating function and preparation method thereof, in particular a kind of polyurethane cement foam thermal insulation fire-retardant material and preparation method thereof.
Background technology
Organic insulation materials such as traditional PS and urethane have the ability of stronger opposing external force, also have advantages such as light weight, thermal conductivity are low, good heat resistance, and utilization extensively in existing energy saving building.Yet ubiquity insulation and the shortcoming that fire prevention can not take into account discharge a large amount of heats, produce a large amount of poison gas when burning, not only can quicken big fire spreading, and cause trapped personnel and rescue personnel's injures and deaths easily.Advantages such as inorganic materials such as traditional rock mineral wool and glass wool have acid and alkali-resistance, corrosion-resistant, stability height, and are ageing-resistant.But show that foam is more crisp, be prone to efflorescence, aspect shortcoming such as intensity is low; Also have aspect shortcomings such as dust and fiber fines, not only polluted air but also easy breed bacteria become the hidden danger that endangers health of people already; And thermal and insulating performance is limited, and range of application is restricted.Under existing situation, through organic materials and inorganic materials are combined, the preparation organic/inorganic composite material has been given play to advantage separately, overcomes deficiency separately, is the important directions of following heat preservation fireproofing material development.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of polyurethane cement foam thermal insulation fire-retardant material and preparation method thereof is provided,, realize fireproof heat insulating through in cement, introducing great amount of bubbles and a spot of urethane.
The present invention realizes through following technical scheme, the present invention includes by weight 50～70 parts of cement, 27～32 parts in water, 1.5～2 parts of whipping agents, 0.2～0.5 part of hardening accelerator, 0.5～1.5 part of water reducer, 5～25 parts of aqurous ployurethanes.
Said cement is selected from one or more in aluminosulfate cement, silicate cement, the sulfate cement.
As a kind of optimal way, said water is that temperature is 30～50 ℃ a warm water.
As a kind of optimal way, said whipping agent is ydrogen peroxide 50 or aluminium powder.
As a kind of optimal way, said hardening accelerator is trolamine or sodium sulfate.
As a kind of optimal way, said water reducer is a naphthalenesulfonate formaldehyde condensation compound.
Said aqurous ployurethane comprises following composition, poly glycol monomethyl ether: glycol ether: the mol ratio of isocyanic ester is (1～4): 1: (1.5～3).
As a kind of optimal way, said isocyanic ester is isophorone two isocyanic acids.
The preparation process of said aqurous ployurethane may further comprise the steps:
(1) with glycol ether after 4 molecular sieves soak, react under the condition of nitrogen protection with isocyanic ester and to make base polyurethane prepolymer for use as, the reaction times of glycol ether and isocyanic ester is 3～5 hours, temperature is at 70～90 ℃;
(2) base polyurethane prepolymer for use as that poly glycol monomethyl ether vacuumizes after the dehydration and step (1) makes is 100～120 ℃ of reaction 4～6h under nitrogen protection; The temperature of product is reduced to 40～50 ℃, make aqurous ployurethane according to solid content 50～60% thin ups.
A kind of preparation method of polyurethane cement foam thermal insulation fire-retardant material may further comprise the steps:
(1) water is added in the cement stirs, until stirring;
(2) aqurous ployurethane is joined in the above-mentioned cement slurry, continue to be stirred to and mix;
(3) water reducer, hardening accelerator and whipping agent are added in the mixture that step (2) forms successively stir, the time respectively is 5～8 minutes;
(4) treat the polyurethane cement foam that the mixture solidified moulding of step (3) promptly makes.
The present invention compares prior art and has the following advantages: polyurethane cement foam thermal insulation fire-retardant material of the present invention; Be to introduce small in a large number, stable, lockedin air space and a spot of urethane in the cement; It is evenly dispersed in the cement matrix, forms polyurethane cement foam thermal insulation fire-retardant material, overcome inorganic materials and be prone to efflorescence; Shortcomings such as intensity is low, heat insulation effect difference, have lightweight, sound insulation, high temperature resistant, Young's modulus is big, advantage such as corrosion-resistant, durable.
Description of drawings
Fig. 1 is the test pattern of embodiment 1 aqurous ployurethane film ir spectra (FT-IR).
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
Present embodiment at first prepares aqurous ployurethane:
(1) with glycol ether after 4 molecular sieves soak 48 h, react under the condition of nitrogen protection with isophorone two isocyanic acids and to make base polyurethane prepolymer for use as, the mol ratio of glycol ether and isophorone two isocyanic acids is 1:1.5, the reaction times is 3h, temperature is at 70 ℃;
(2) vacuumize the base polyurethane prepolymer for use as 100 ℃ of reaction 4h under nitrogen protection that make with step (1) behind the dehydration 2h under 110 ℃ of the poly glycol monomethyl ethers; The temperature of product is reduced to 40 ℃; Make aqurous ployurethane according to solid content 50～60% thin ups, the mol ratio of poly glycol monomethyl ether and glycol ether is 1:1.
(Bruker Vector-22) detects the structural characterization of the aqurous ployurethane that present embodiment is made, and the urethane charateristic avsorption band is respectively among Fig. 1: 3310 cm by IR -1Stretching vibration peak, 1560 cm for N-H -1Flexural vibration peak, 1712 cm for N-H -1Be C=O stretching vibration peak, 1118 cm -1Be the C-O-C stretching vibration peak.
A kind of preparation method of polyurethane cement foam thermal insulation fire-retardant material may further comprise the steps:
(1) 27 parts in 30 ℃ warm water that will be by weight adds in 50 parts of the aluminosulfate cements and stirs, until stirring;
(2) with above-mentioned aqurous ployurethane by weight 5 parts join in the above-mentioned cement slurry, continue to be stirred to and mix;
(3) 1.5 parts in 0.2 part of 0.5 part of naphthalenesulfonate formaldehyde condensation compound, trolamine that will be by weight and ydrogen peroxide 50 add successively in the mixture that step (2) forms and stir, and the time respectively is 5 minutes;
(4) fire-retardant heat-insulation material that step (3) is stirred injects mould, puts into the maintenance of cement standard maintaining box.With reference to JG 158-2004 standard polyurethane cement foam thermal insulation fire-retardant material thermal conductivity and ultimate compression strength and dry density are tested; With reference to GB/T 20473-2006 standard combustionproperty is tested.Ultimate compression strength, thermal conductivity, dry density and the combustionproperty grade that records 28 days polyurethane cement foam thermal insulation fire-retardant materials is respectively 0.53MPa, 213 kg/m3,0.045 W (mK) and A level.
Embodiment 2
Present embodiment at first prepares aqurous ployurethane:
(1) with glycol ether after 4 molecular sieves soak 48 h, react under the condition of nitrogen protection with isophorone two isocyanic acids and to make base polyurethane prepolymer for use as, the mol ratio of glycol ether and isophorone two isocyanic acids is 1:3, the reaction times is 5h, temperature is at 90 ℃;
(2) vacuumize the base polyurethane prepolymer for use as 120 ℃ of reaction 6h under nitrogen protection that make with step (1) behind the dehydration 3h under 110 ℃ of the poly glycol monomethyl ethers; The temperature of product is reduced to 50 ℃; Make aqurous ployurethane according to solid content 50～60% thin ups, the mol ratio of poly glycol monomethyl ether and glycol ether is 4:1.
A kind of preparation method of polyurethane cement foam thermal insulation fire-retardant material may further comprise the steps:
(1) 32 parts in 50 ℃ warm water that will be by weight adds in 70 parts of the silicate cements and stirs, until stirring;
(2) with above-mentioned aqurous ployurethane by weight 25 parts join in the above-mentioned cement slurry, continue to be stirred to and mix;
(3) 2 parts of 0.5 part in 1.5 parts of naphthalenesulfonate formaldehyde condensation compounds, sodium sulfate that will be by weight and aluminium powders add successively in the mixture that step (2) forms and stir, and the time respectively is 8 minutes;
(4) fire-retardant heat-insulation material that step (3) is stirred injects mould, puts into the maintenance of cement standard maintaining box.With reference to JG 158-2004 standard polyurethane cement foam thermal insulation fire-retardant material thermal conductivity and ultimate compression strength and dry density are tested; With reference to GB/T 20473-2006 standard combustionproperty is tested.The ultimate compression strength, thermal conductivity, dry density and the combustionproperty grade that record 28 days polyurethane cement foam thermal insulation fire-retardant materials are respectively 0.73MPa, 205kg/m 3, 0.041W (mK) and A level.
Embodiment 3
Present embodiment at first prepares aqurous ployurethane:
(1) with glycol ether after 4 molecular sieves soak 48 h, react under the condition of nitrogen protection with isophorone two isocyanic acids and to make base polyurethane prepolymer for use as, the mol ratio of glycol ether and isophorone two isocyanic acids is 1:2, the reaction times is 4h, temperature is at 80 ℃;
(2) vacuumize the base polyurethane prepolymer for use as 110 ℃ of reaction 5h under nitrogen protection that make with step (1) behind the dehydration 2.5h under 110 ℃ of the poly glycol monomethyl ethers; The temperature of product is reduced to 45 ℃; Make aqurous ployurethane according to solid content 50～60% thin ups, the mol ratio of poly glycol monomethyl ether and glycol ether is 2:1.
A kind of preparation method of polyurethane cement foam thermal insulation fire-retardant material may further comprise the steps:
(1) 30 parts in 40 ℃ warm water that will be by weight adds in 60 parts of the sulfate cements and stirs, until stirring;
(2) with above-mentioned aqurous ployurethane by weight 10 parts join in the above-mentioned cement slurry, continue to be stirred to and mix;
(3) 1.7 parts of 0.3 part in 1 part of naphthalenesulfonate formaldehyde condensation compound, sodium sulfate that will be by weight and aluminium powders add successively in the mixture that step (2) forms and stir, and the time respectively is 6 minutes;
(4) fire-retardant heat-insulation material that step (3) is stirred injects mould, puts into the maintenance of cement standard maintaining box.With reference to JG 158-2004 standard polyurethane cement foam thermal insulation fire-retardant material thermal conductivity and ultimate compression strength and dry density are tested; With reference to GB/T 20473-2006 standard combustionproperty is tested.The ultimate compression strength, thermal conductivity, dry density and the combustionproperty grade that record 28 days polyurethane cement foam thermal insulation fire-retardant materials are respectively 0.68MPa, 198kg/m 3, 0.043W (mK) and A level.
Embodiment 4
Present embodiment at first prepares aqurous ployurethane:
(1) with glycol ether after 4 molecular sieves soak 48 h, react under the condition of nitrogen protection with isophorone two isocyanic acids and to make base polyurethane prepolymer for use as, the mol ratio of glycol ether and isophorone two isocyanic acids is 1:2.5, the reaction times is 3.5h, temperature is at 75 ℃;
(2) vacuumize the base polyurethane prepolymer for use as 115 ℃ of reaction 4.5h under nitrogen protection that make with step (1) behind the dehydration 2h under 110 ℃ of the poly glycol monomethyl ethers; The temperature of product is reduced to 42 ℃; Make aqurous ployurethane according to solid content 50～60% thin ups, the mol ratio of poly glycol monomethyl ether and glycol ether is 3:1.
A kind of preparation method of polyurethane cement foam thermal insulation fire-retardant material may further comprise the steps:
(1) 28 parts in 45 ℃ warm water that will be by weight adds in 65 parts of the sulfate cements and stirs, until stirring;
(2) with above-mentioned aqurous ployurethane by weight 20 parts join in the above-mentioned cement slurry, continue to be stirred to and mix;
(3) 1.8 parts in 0.4 part of 0.9 part of naphthalenesulfonate formaldehyde condensation compound, trolamine that will be by weight and ydrogen peroxide 50 add successively in the mixture that step (2) forms and stir, and the time respectively is 7 minutes;
(4) fire-retardant heat-insulation material that step (3) is stirred injects mould, puts into the maintenance of cement standard maintaining box.With reference to JG 158-2004 standard polyurethane cement foam thermal insulation fire-retardant material thermal conductivity and ultimate compression strength and dry density are tested; With reference to GB/T 20473-2006 standard combustionproperty is tested.The ultimate compression strength, thermal conductivity, dry density and the combustionproperty grade that record 28 days polyurethane cement foam thermal insulation fire-retardant materials are respectively 0.88MPa, 210kg/m 3, 0.042W (mK) and A level.

Claims (10)

1. a polyurethane cement foam thermal insulation fire-retardant material is characterized in that, comprises by weight 50～70 parts of cement, 27～32 parts in water, 1.5～2 parts of whipping agents, 0.2～0.5 part of hardening accelerator, 0.5～1.5 part of water reducer, 5～25 parts of aqurous ployurethanes.
2. polyurethane cement foam thermal insulation fire-retardant material according to claim 1, it is characterized in that: said cement is selected from one or more in aluminosulfate cement, silicate cement, the sulfate cement.
3. polyurethane cement foam thermal insulation fire-retardant material according to claim 1 is characterized in that: said water is that temperature is 30～50 ℃ a warm water.
4. polyurethane cement foam thermal insulation fire-retardant material according to claim 1 is characterized in that: said whipping agent is ydrogen peroxide 50 or aluminium powder.
5. polyurethane cement foam thermal insulation fire-retardant material according to claim 1 is characterized in that: said hardening accelerator is trolamine or sodium sulfate.
6. polyurethane cement foam thermal insulation fire-retardant material according to claim 1 is characterized in that: said water reducer is a naphthalenesulfonate formaldehyde condensation compound.
7. polyurethane cement foam thermal insulation fire-retardant material according to claim 1, it is characterized in that: said aqurous ployurethane comprises following composition, poly glycol monomethyl ether: glycol ether: the mol ratio of isocyanic ester is (1～4): 1: (1.5～3).
8. polyurethane cement foam thermal insulation fire-retardant material according to claim 7 is characterized in that: said isocyanic ester is isophorone two isocyanic acids.
9. polyurethane cement foam thermal insulation fire-retardant material according to claim 7 is characterized in that, the preparation process of said aqurous ployurethane may further comprise the steps:
(1) with glycol ether after 4 molecular sieves soak, react under the condition of nitrogen protection with isocyanic ester and to make base polyurethane prepolymer for use as, the reaction times of glycol ether and isocyanic ester is 3～5 hours, temperature is at 70～90 ℃;
(2) base polyurethane prepolymer for use as that poly glycol monomethyl ether vacuumizes after the dehydration and step (1) makes is 100～120 ℃ of reaction 4～6h under nitrogen protection; The temperature of product is reduced to 40～50 ℃, make aqurous ployurethane according to solid content 50～60% thin ups.
10. the preparation method of a polyurethane cement foam thermal insulation fire-retardant material as claimed in claim 1 is characterized in that, may further comprise the steps:
(1) water is added in the cement stirs, stir;
(2) aqurous ployurethane is joined in the above-mentioned cement slurry, continue to be stirred to and mix;
(3) water reducer, hardening accelerator and whipping agent are added in the mixture that step (2) forms successively stir, the time respectively is 5～8 minutes;
(4) treat the polyurethane cement foam that the mixture solidified moulding of step (3) promptly makes.
CN2012102196277A 2012-06-29 2012-06-29 Insulated fireproof material of polyurethane cement foam and preparation method of insulated fireproof material Pending CN102701687A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261766A (en) * 2014-09-29 2015-01-07 句容金猴机械研究所有限公司 High-toughness mould pressing tile and preparation method thereof
CN104291756A (en) * 2014-09-29 2015-01-21 句容金猴机械研究所有限公司 High-strength thermal insulation mould pressing tile and manufacturing method thereof
CN106565167A (en) * 2016-07-15 2017-04-19 中南大学 Polyurethane and foamed cement microscopically-composite heat insulating material and preparation method therefor
CN106747590A (en) * 2017-02-22 2017-05-31 中南大学 A kind of foaming method of polyurethane with cement In-situ reaction and its application
CN107344839A (en) * 2017-08-15 2017-11-14 重庆市佰恒科技有限公司 A kind of building heat preservation fire proofing material and preparation method thereof
CN109734870A (en) * 2018-12-26 2019-05-10 哈尔滨工程大学 A kind of preparation method of water-fast pressure-resistant plugging material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563174A (en) * 2004-04-08 2005-01-12 武汉鲲鹏节能材料有限公司 Waterproof heat insulated thermal-protection material
CN101412610A (en) * 2008-11-19 2009-04-22 建筑材料工业技术监督研究中心 High performance polymer cement foam material and preparation thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563174A (en) * 2004-04-08 2005-01-12 武汉鲲鹏节能材料有限公司 Waterproof heat insulated thermal-protection material
CN101412610A (en) * 2008-11-19 2009-04-22 建筑材料工业技术监督研究中心 High performance polymer cement foam material and preparation thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261766A (en) * 2014-09-29 2015-01-07 句容金猴机械研究所有限公司 High-toughness mould pressing tile and preparation method thereof
CN104291756A (en) * 2014-09-29 2015-01-21 句容金猴机械研究所有限公司 High-strength thermal insulation mould pressing tile and manufacturing method thereof
CN106565167A (en) * 2016-07-15 2017-04-19 中南大学 Polyurethane and foamed cement microscopically-composite heat insulating material and preparation method therefor
CN106565167B (en) * 2016-07-15 2019-03-26 中南大学 A kind of polyurethane and the microcosmic compound thermal insulation material and preparation method thereof of foamed cement
CN106747590A (en) * 2017-02-22 2017-05-31 中南大学 A kind of foaming method of polyurethane with cement In-situ reaction and its application
CN107344839A (en) * 2017-08-15 2017-11-14 重庆市佰恒科技有限公司 A kind of building heat preservation fire proofing material and preparation method thereof
CN109734870A (en) * 2018-12-26 2019-05-10 哈尔滨工程大学 A kind of preparation method of water-fast pressure-resistant plugging material
CN109734870B (en) * 2018-12-26 2021-09-28 哈尔滨工程大学 Preparation method of water-resistant pressure-resistant plugging material

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