CN110408081A - A kind of flame retardant composite material for building and preparation method thereof - Google Patents

A kind of flame retardant composite material for building and preparation method thereof Download PDF

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Publication number
CN110408081A
CN110408081A CN201910725161.XA CN201910725161A CN110408081A CN 110408081 A CN110408081 A CN 110408081A CN 201910725161 A CN201910725161 A CN 201910725161A CN 110408081 A CN110408081 A CN 110408081A
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composite material
flame retardant
building
retardant composite
graphite
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唐小燕
薛万里
郭川川
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Henan Zhongbai Fireproof Coatings Technology Co Ltd
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Henan Zhongbai Fireproof Coatings Technology Co Ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/36Sulfur-, selenium-, or tellurium-containing compounds
    • C08K5/41Compounds containing sulfur bound to oxygen
    • C08K5/42Sulfonic acids; Derivatives thereof
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/08Ingredients agglomerated by treatment with a binding agent
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00Coating compositions based on 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 alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C09D129/02Homopolymers or copolymers of unsaturated alcohols
    • C09D129/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant

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Abstract

The present invention relates to building product fields more particularly to a kind of flame retardant composite material for building and preparation method thereof.The flame retardant composite material for building, in parts by weight, including at least following components: 50~100 parts of calcium carbonate;1~5 part of graphite;1~5 part of alpha-olefin sodium sulfonate;1~10 part of calcium sulphate retarder;1~3 part of filler.The preparation method of the flame retardant composite material for building, at least includes the following steps: weighing calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler according to corresponding parts by weight, after mixing, obtains flame retardant composite material for building.

Description

A kind of flame retardant composite material for building and preparation method thereof
Technical field
The present invention relates to building product fields more particularly to a kind of flame retardant composite material for building and preparation method thereof.
Background technique
Fire retardant is one of most commonly used auxiliary agent of industrial application, and is produced with the closely bound up chemical industry of people's lives One of product.Addition fire retardant is the most direct effective method of flame retardance of polymer processing.There are two types of modes for addition fire retardant: directly adding Add (additive flame retardant) and by chemical reaction addition (reactive flame retardant).Halogen can be divided into according to the component difference of fire retardant Flame retardant, organic phosphorus nitrogen based flame retardant, expansion type flame retardant and inorganic fire retardants etc..decagram Commissioning
For halogen based flame retardant, with the promulgation of relevant laws and regulations, application range receives certain restriction, but It is still to there is a large amount of halogen based flame retardant using in China market, wherein predominantly brominated flame retardant, such as tetrabromobisphenol A Deng.In actual application, halogen based flame retardant is usually used in compounding composition cooperative flame retardant system with other synergists, such as Halogen/antimony cooperative system etc..
Thus, it is also very desirable to by the improvement of technique, to develop a while there is fire-retardant and anti-powdering effect build It builds and uses flame retardant composite material.
Summary of the invention
In order to solve the above-mentioned technical problem, the first aspect of the invention provides a kind of flame retardant composite material for building, The flame retardant composite material for building includes at least following components in parts by weight:
As a preferred technical solution of the present invention, the flame retardant composite material for building at least wraps in parts by weight Include following components:
As a preferred technical solution of the present invention, the flame retardant composite material for building at least wraps in parts by weight Include following components:
As a preferred technical solution of the present invention, the calcium carbonate is nanometer calcium carbonate.
As a preferred technical solution of the present invention, the graphite is expanded graphite.
As a preferred technical solution of the present invention, the expanded graphite is composite material intercalated graphite;
The structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A and the C are independently selected from: appointing in maleic anhydride modified polypropylene, end carboxyl super branched polyester It anticipates one kind.
As a preferred technical solution of the present invention, the B is selected from: aminosilane coupling agent modifying nanometer titanium dioxide Silicon;The A is selected from: maleic anhydride modified polypropylene;The C is selected from: end carboxyl super branched polyester.
As a preferred technical solution of the present invention, the calcium sulphate retarder is selected from: citric acid, sodium polyphosphate, boron It is one or more in sand.
As a preferred technical solution of the present invention, the filler is selected from: nano silica, nano aluminium oxide, cunning Mountain flour, montmorillonite, calcium oxide, wollastonite, any one or a few the mixing in mica.
The second aspect of the invention provides a kind of preparation method of flame retardant composite material for building, includes at least following Step:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
The above-mentioned of the application and other features, aspects and advantages are more readily understood with reference to following detailed description.
Specific embodiment
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily to understand Bright content.Unless otherwise defined, all technologies used herein and scientific term have common with fields of the present invention The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... preparation " it is synonymous with "comprising".Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that cover non-exclusionism includes.For example, the combination comprising listed elements Object, step, method, product or device are not necessarily limited to those elements, but may include not expressly listed other elements or Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this Phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative normal Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body, It is only limited to element described in the clause;Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to 5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end Value and all integers and score in the range.
Singular includes that plural number discusses object, unless the context clearly dictates otherwise." optional " or it is " any It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and The situation that event does not occur.
Approximate term in specification and claims is used to modify quantity, and it is specific to indicate that the present invention is not limited to this Quantity further includes the acceptable modified part without will lead to the change of dependency basis this function close with the quantity.Phase It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, approximate Term likely corresponds to the precision of the instrument of measurement numerical value.In present specification and claims, range limits can be with Combination and/or exchange, these ranges if not stated otherwise include all subranges contained therebetween.
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component (i.e. frequency of occurrence) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and odd number The element or component of form also include plural form, unless the obvious purport of the quantity refers to singular.
In order to solve the above-mentioned technical problem, the first aspect of the invention provides a kind of flame retardant composite material for building, The flame retardant composite material for building includes at least following components in parts by weight:
In a preferred embodiment, the flame retardant composite material for building includes at least following in parts by weight Component:
In a preferred embodiment, the flame retardant composite material for building includes at least following in parts by weight Component:
Calcium carbonate
Term " calcium carbonate " is a kind of inorganic compound, is commonly called as: lime stone, lime stone, mountain flour, marble etc..Main component: Calcite, chemical formula are CaCO3, it is in neutrality, is substantially insoluble in, is dissolved in hydrochloric acid.It is Common materials on the earth, is present in It is also the main component of animal skeleton or shell in the rocks such as aragonite, calcite, chalk, limestone, marble, calcareous tufa.
In the application, used " calcium carbonate " is not particularly limited, and can be the calcium carbonate of any form.
In a preferred embodiment, the calcium carbonate is nanometer calcium carbonate.
The nanometer calcium carbonate is also known as super fine calcium carbonate;
The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to industrial (Suzhou) Co., Ltd of ultra micro, product grade LD- 1000C。
Graphite
Term " graphite " is a kind of allotrope of elemental carbon, and it is former that the periphery of each carbon atom links the other three carbon Son (arrangement mode is in cellular multiple hexagons) constitutes covalent molecule with Covalent bonding together.In the application, used stone Ink is the graphite of any one commercially available trade mark.
In a preferred embodiment, the graphite is expanded graphite.
Term " expanded graphite " is that graphite obtains after intercalation modifying.
In a preferred embodiment, the expanded graphite is composite material intercalated graphite;
The structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A and the C are independently selected from: appointing in maleic anhydride modified polypropylene, end carboxyl super branched polyester It anticipates one kind.
In a preferred embodiment, the structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A is selected from: maleic anhydride modified polypropylene;
The C is selected from: end carboxyl super branched polyester.
In a preferred embodiment, the preparation method of the aminosilane coupling agent modifying nano silica is extremely Less the following steps are included:
In the reactor, solvent 200ml toluene is added and then 12g nano silica, ultrasonic disperse 30min is added The triethylamine solution that 30mL volumetric concentration is 10% is added in 5g amino silicane coupling agent, and the back flow reaction 3h at 100 DEG C is filtered, Ethanol washing 3 times, it is dried to obtain aminosilane coupling agent modifying nano silica.
The amino silicane coupling agent is γ-(ethylenediamine base) propyl trimethoxy silicane;The nano silica purchase In Nanjing Xian Feng Nono-material Science & Technology Ltd., the trade mark of product is XFF11;The nano silica belongs to monodisperse Jie Hole silicon dioxide nanosphere is starlike.
In a preferred embodiment, in the maleic anhydride modified polypropylene, maleic anhydride with it is polyacrylic heavy Amount is than being 1:(30~50).
In a preferred embodiment, the maleic anhydride modified polypropylene the preparation method comprises the following steps: by polypropylene and Maleic anhydride mixing resulting mixture, is added in pyroreaction kettle, is stirred melting, and initiator is added after melting, described Initiator is cumyl peroxide, and the weight ratio of the polypropylene and cumyl peroxide is 100:1, is stirred under melting 2h obtains maleic anhydride modified polypropylene.
The end carboxyl super branched polyester is purchased from Wuhan hyperbranched resin Science and Technology Ltd..
In a preferred embodiment, the preparation method of the A-B-C, at least includes the following steps:
The maleic anhydride modified polypropylene of 10g is dissolved in solvent xylene, 50g amino silicane coupling agent is then added Reaction temperature after stirring, is increased to 70 DEG C by modified manometer silicon dioxide, is then added into system end carboxyl super branched poly- Ester is stirred dissolution again, and then into system, the DMAP of the DCC and 0.5g of addition 1g are as catalyst, at 40 DEG C, into Reactant is carried out deionized water and washed 3 times, ethanol washing 3 times, obtains A-B-C after dry by row reaction 6h.
In a preferred embodiment, the preparation method of the expanded graphite at least includes the following steps:
The graphite for weighing 100g is added in the deionized water of 1000g, and 5g neopelex, 30 points of ultrasound is added Clock, the power of ultrasonic disperse are 150W, obtain graphite suspension;Then A-B-C is added into graphite suspension again, increases reaction To 50 DEG C, the ultrasound 2h at 40 DEG C after filtering, is washed with deionized 3 times, expanded graphite is obtained after vacuum drying temperature.
Alpha-olefin sodium sulfonate
In the application, used alpha-olefin sodium sulfonate is not particularly limited, in the application, the alpha-olefin sulphur that uses Sour sodium is commercially available acquisition.
Calcium sulphate retarder
In the application, used calcium sulphate retarder is not particularly limited.
In a preferred embodiment, the calcium sulphate retarder is selected from: citric acid, sodium polyphosphate, one in borax Kind is a variety of.
Filler
In the present invention, the filler is not particularly limited.
In a preferred embodiment, the filler is selected from: nano silica, nano aluminium oxide, talcum powder, illiteracy De- soil, calcium oxide, wollastonite, any one or a few the mixing in mica.
The second aspect of the invention provides a kind of preparation method of flame retardant composite material for building, includes at least following Step:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field The some nonessential modifications and adaptations made according to the content of aforementioned present invention, still fall within protection scope of the present invention.
In addition, if without other explanations, it is raw materials used to be all commercially available, it is purchased from traditional Chinese medicines chemical reagent.
Embodiment 1:
The embodiment of the present invention 1 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 2:
The embodiment of the present invention 2 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 3:
The embodiment of the present invention 3 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 4:
The embodiment of the present invention 4 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 5:
The embodiment of the present invention 5 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 6:
The embodiment of the present invention 6 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is expanded graphite;
The expanded graphite is composite material intercalated graphite;
The structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A is selected from: maleic anhydride modified polypropylene;
The C is selected from: maleic anhydride modified polypropylene;
The preparation method of the aminosilane coupling agent modifying nano silica, at least includes the following steps:
In the reactor, solvent 200ml toluene is added and then 12g nano silica, ultrasonic disperse 30min is added The triethylamine solution that 30mL volumetric concentration is 10% is added in 5g amino silicane coupling agent, and the back flow reaction 3h at 100 DEG C is filtered, Ethanol washing 3 times, it is dried to obtain aminosilane coupling agent modifying nano silica.
The amino silicane coupling agent is γ-(ethylenediamine base) propyl trimethoxy silicane;The nano silica purchase In Nanjing Xian Feng Nono-material Science & Technology Ltd., the trade mark of product is XFF11;The nano silica belongs to monodisperse Jie Hole silicon dioxide nanosphere is starlike.
The preparation method of the maleic anhydride modified polypropylene, at least includes the following steps:
It is added to polypropylene and maleic anhydride mixing resulting mixture in pyroreaction kettle, melting is stirred, after melting Add initiator, the initiator is cumyl peroxide, and the weight ratio of the polypropylene and cumyl peroxide is 100:1 stirs 2h under melting, obtains maleic anhydride modified polypropylene.
In the maleic anhydride modified polypropylene, maleic anhydride and polyacrylic weight ratio are 1:30.The polypropylene is Homopolypropylene.
The preparation method of the A-B-C, at least includes the following steps:
The maleic anhydride modified polypropylene of 20g is dissolved in solvent xylene, 50g amino silicane coupling agent is then added Reaction temperature after stirring, is increased to 70 DEG C by modified manometer silicon dioxide, is then added the DCC's and 1g of 1g into system DMAP is as catalyst, at 40 DEG C, carries out reaction 6h, and reactant is carried out deionized water and is washed 3 times, ethanol washing 3 times, is done A-B-C is obtained after dry.
The preparation method of the expanded graphite at least includes the following steps:
The graphite for weighing 100g is added in the deionized water of 1000g, and 5g neopelex, 30 points of ultrasound is added Clock, the power of ultrasonic disperse are 150W, obtain graphite suspension;Then A-B-C is added into graphite suspension again, increases reaction To 50 DEG C, the ultrasound 2h at 40 DEG C after filtering, is washed with deionized 3 times, expanded graphite is obtained after vacuum drying temperature.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 7:
The embodiment of the present invention 7 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is expanded graphite;
The expanded graphite is composite material intercalated graphite;
The structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A is selected from: end carboxyl super branched polyester;
The C is selected from: end carboxyl super branched polyester;
The preparation method of the aminosilane coupling agent modifying nano silica at least includes the following steps:
In the reactor, solvent 200ml toluene is added and then 12g nano silica, ultrasonic disperse 30min is added The triethylamine solution that 30mL volumetric concentration is 10% is added in 5g amino silicane coupling agent, and the back flow reaction 3h at 100 DEG C is filtered, Ethanol washing 3 times, it is dried to obtain aminosilane coupling agent modifying nano silica.
The amino silicane coupling agent is γ-(ethylenediamine base) propyl trimethoxy silicane;The nano silica purchase In Nanjing Xian Feng Nono-material Science & Technology Ltd., the trade mark of product is XFF11;The nano silica belongs to monodisperse Jie Hole silicon dioxide nanosphere is starlike.
The end carboxyl super branched polyester is purchased from Wuhan hyperbranched resin Science and Technology Ltd..
The preparation method of the A-B-C, at least includes the following steps:
The end carboxyl super branched polyester of 20g is dissolved in solvent xylene, 50g aminosilane coupling agent modifying is then added Reaction temperature after stirring, is increased to 80 DEG C by nano silica, and the DMAP that the DCC and 1g of 1g is then added into system makees Reaction 6h is carried out at 40 DEG C for catalyst, reactant is subjected to deionized water and is washed 3 times, ethanol washing 3 times, is obtained after dry To A-B-C.
The preparation method of the expanded graphite at least includes the following steps:
The graphite for weighing 100g is added in the deionized water of 1000g, and 5g neopelex, 30 points of ultrasound is added Clock, the power of ultrasonic disperse are 150W, obtain graphite suspension;Then A-B-C is added into graphite suspension again, increases reaction To 50 DEG C, the ultrasound 2h at 40 DEG C after filtering, is washed with deionized 3 times, expanded graphite is obtained after vacuum drying temperature.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Embodiment 8:
The embodiment of the present invention 8 provides a kind of flame retardant composite material for building, the flame retardant composite material for building, with Parts by weight meter includes at least following components:
The calcium carbonate is nanometer calcium carbonate;The nanometer calcium carbonate is commercially available acquisition, is purchased from vertical up to ultra micro industry (Soviet Union State) Co., Ltd, product grade LD-1000C.
The graphite is expanded graphite;
The expanded graphite is composite material intercalated graphite;
The structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A is selected from: maleic anhydride modified polypropylene;
The C is selected from: end carboxyl super branched polyester;
The preparation method of the aminosilane coupling agent modifying nano silica at least includes the following steps:
In the reactor, solvent 200ml toluene is added and then 12g nano silica, ultrasonic disperse 30min is added The triethylamine solution that 30mL volumetric concentration is 10% is added in 5g amino silicane coupling agent, and the back flow reaction 3h at 100 DEG C is filtered, Ethanol washing 3 times, it is dried to obtain aminosilane coupling agent modifying nano silica.
The amino silicane coupling agent is γ-(ethylenediamine base) propyl trimethoxy silicane;The nano silica purchase In Nanjing Xian Feng Nono-material Science & Technology Ltd., the trade mark of product is XFF11;The nano silica belongs to monodisperse Jie Hole silicon dioxide nanosphere is starlike.
The maleic anhydride modified polypropylene the preparation method comprises the following steps: by polypropylene and maleic anhydride mixing resulting mixture, add Entering into pyroreaction kettle, be stirred melting, initiator is added after melting, the initiator is cumyl peroxide, The weight ratio of the polypropylene and cumyl peroxide is 100:1, stirs 2h under melting, obtains maleic anhydride modified poly- third Alkene.
In the maleic anhydride modified polypropylene, maleic anhydride and polyacrylic weight ratio are 1:40.
The end carboxyl super branched polyester is purchased from Wuhan hyperbranched resin Science and Technology Ltd..
The preparation method of the A-B-C, at least includes the following steps:
The maleic anhydride modified polypropylene of 10g is dissolved in solvent xylene, 50g amino silicane coupling agent is then added Reaction temperature after stirring, is increased to 70 DEG C by modified manometer silicon dioxide, is then added into system end carboxyl super branched poly- Ester is stirred dissolution again, and then into system, the DMAP of the DCC and 0.5g of addition 1g are as catalyst, at 40 DEG C, into Reactant is carried out deionized water and washed 3 times, ethanol washing 3 times, obtains A-B-C after dry by row reaction 6h.
The preparation method of the expanded graphite at least includes the following steps:
The graphite for weighing 100g is added in the deionized water of 1000g, and 5g neopelex, 30 points of ultrasound is added Clock, the power of ultrasonic disperse are 150W, obtain graphite suspension;Then A-B-C is added into graphite suspension again, increases reaction To 50 DEG C, the ultrasound 2h at 40 DEG C after filtering, is washed with deionized 3 times, expanded graphite is obtained after vacuum drying temperature.
The graphite is crystalline flake graphite, is purchased from Yichang Xincheng Graphite Co., Ltd..
The calcium sulphate retarder is citric acid;
The filler is nano silica, is purchased from Nanjing Tian Hang new material Co., Ltd, product grade are as follows: TSP- H10。
The preparation method of flame retardant composite material for building, at least includes the following steps:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed After uniformly, flame retardant composite material for building is obtained.
Comparative example 1:
Comparative example 1 is with embodiment 8, the difference lies in that A-B-C is replaced with B.
Comparative example 2:
Comparative example 2 is with embodiment 8, the difference lies in that A-B-C is replaced with nano silica.
Comparative example 3:
Comparative example 3 is with embodiment 8, the difference lies in that A-B-C is replaced with silane coupling agent γ-(ethylenediamine base) propyl Trimethoxy silane.
Comparative example 4:
Comparative example 4 is with embodiment 8, the difference lies in that A-B-C is replaced with maleic anhydride modified polypropylene.
Comparative example 5:
Comparative example 5 is with embodiment 8, the difference lies in that A-B-C is replaced with polypropylene.
Comparative example 6:
Comparative example 6 is with embodiment 8, the difference lies in that A-B-C is replaced with maleic acid.
Comparative example 7:
Comparative example 7 is with embodiment 8, the difference lies in that A-B-C is replaced with end carboxyl super branched polyester.
Comparative example 8:
Comparative example 8 is with embodiment 8, the difference lies in that A-B-C is replaced with ammonium polyphosphate.
Comparative example 9:
Comparative example 9 is with embodiment 8, the difference lies in that expanded graphite is replaced with ammonium polyphosphate.
Comparative example 10:
Comparative example 10 is with embodiment 8, the difference lies in that expanded graphite is replaced with aluminium hydroxide.
The product that Examples 1 to 8 and comparative example 1~10 are obtained respectively and tap water according to weight ratio be 1:1 ratio Example is mixed, and after mixing evenly, is then mixed with 803 coating;Wherein, 803 coating and environmental-protection flame-retardant additive Weight ratio is 10:1.It is coated on plastic strip respectively, carries out test flame retardant property and chalking resistance energy.
Performance evaluation
1, flame retardant property is tested according to UL94 horizontal vertical combustion method.
Flame retardant property test tests flame retardant property at normal temperatures and pressures and at 200 DEG C respectively respectively.
2, for chalk rating referring to ISO4628-7 is pressed, dusting degree and grade are shown in Table 1.
Chalk rating test tests powder performance at normal temperatures and pressures and under 100% humidity respectively.
1 chalk rating of table
Grade Dusting degree
0 Without dusting
1 It is very slight, it tries that micro particle can be observed on cloth
2 Slightly, it tries that a small amount of particle can be observed on cloth
3 Obviously, it tries that more particle can be observed on cloth
4 It is heavier, it tries that many particles can be observed on cloth
5 Seriously, it tries that a large amount of particle can be observed on cloth or template appearance is show-through
2 characterization test of table
Example above-mentioned is merely illustrative, and is used to explain the present invention some features of the method.Appended right is wanted The range as wide as possible for being intended to require to be contemplated that is sought, and embodiments as presented herein is only according to all possible implementation The explanation of the embodiment of the combined selection of example.Therefore, the purpose of applicant is that the attached claims are not illustrated this hair The exemplary selectional restriction of bright feature.Some numberical ranges used also include sub- model in the claims It encloses, the variation in these ranges should also be construed to be covered by the attached claims in the conceived case.

Claims (10)

1. a kind of flame retardant composite material for building, which is characterized in that the flame retardant composite material for building, in parts by weight, until Less include following components:
2. flame retardant composite material for building as described in claim 1, which is characterized in that the flame retardant composite material for building, In parts by weight, following components is included at least:
3. flame retardant composite material for building as claimed in claim 2, which is characterized in that the flame retardant composite material for building, In parts by weight, following components is included at least:
4. flame retardant composite material for building as described in claim 1, which is characterized in that the calcium carbonate is nanometer calcium carbonate.
5. flame retardant composite material for building as described in claim 1, which is characterized in that the graphite is expanded graphite.
6. flame retardant composite material for building as claimed in claim 5, which is characterized in that the expanded graphite is inserted for composite material Layer graphite;
The structural formula of the composite material are as follows: A-B-C;
The B is selected from: aminosilane coupling agent modifying nano silica;
The A and the C are independently selected from: any one in maleic anhydride modified polypropylene, end carboxyl super branched polyester Kind.
7. flame retardant composite material for building as claimed in claim 6, which is characterized in that the B is selected from: amino silicane coupling agent Modified manometer silicon dioxide;The A is selected from: maleic anhydride modified polypropylene;The C is selected from: end carboxyl super branched polyester.
8. flame retardant composite material for building as described in claim 1, which is characterized in that the calcium sulphate retarder is selected from: It is citric acid, sodium polyphosphate, one or more in borax.
9. flame retardant composite material for building as claimed in claim 9, which is characterized in that the filler is selected from: nanometer titanium dioxide Silicon, nano aluminium oxide, talcum powder, montmorillonite, calcium oxide, wollastonite, any one or a few the mixing in mica.
10. the preparation method of the flame retardant composite material for building as described in claim 1~9, which is characterized in that include at least with Lower step:
Calcium carbonate, graphite, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is uniformly mixed Afterwards, flame retardant composite material for building is obtained.
CN201910725161.XA 2019-08-07 2019-08-07 A kind of flame retardant composite material for building and preparation method thereof Pending CN110408081A (en)

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Inventor after: Xue Wanli

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Inventor before: Guo Chuanchuan