CN110330254A - One kind black feed composition for building and preparation method thereof - Google Patents
One kind black feed composition for building and preparation method thereof Download PDFInfo
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- CN110330254A CN110330254A CN201910725400.1A CN201910725400A CN110330254A CN 110330254 A CN110330254 A CN 110330254A CN 201910725400 A CN201910725400 A CN 201910725400A CN 110330254 A CN110330254 A CN 110330254A
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- building
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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Abstract
A kind of black feed composition for building, the black feed composition for building, in parts by weight, including at least following components: 50~100 parts of calcium carbonate；1~10 part of graphite；1~3 part of graphene；1~5 part of alpha-olefin sodium sulfonate；1~10 part of calcium sulphate retarder；1~3 part of filler.
Description
Technical field
The present invention relates to building product fields, more particularly to a kind of black feed composition for building and preparation method thereof.
Technical background
Fire proofing be able to suppress or retardation burning and oneself be not easy to burning material, be widely used in taking
The fields such as dress, petroleum, chemical industry, metallurgy, shipbuilding, fire-fighting, national defence.Fire proofing includes organic fire proofing and inorganic fire-retarded material
Material.Wherein, organic fire-resisting material general types have following several: (1) organohalogen compounds.Predominantly bromide, there are commonly ten
Bromo biphenyl acid (DBDPO), tetrabromobisphenol A (TBBPA), brominated Polystyrene (BPS) etc..Chloride only has chlorinated paraffin and chlorination
Polyethylene is applied.Halide often cooperates with use with antimony oxide or phosphide.(2) organic phosphorus compound.It can be divided into inorganic
Two class of phosphorus and halogenated phosphorus.Halogen phosphorus is mainly phosphoric acid class such as triphen (TPP) etc..Halogen phosphorus need to cooperate with addition with phosphorus Halides.It is halogenated
The intramolecular of phosphorus contains two kinds of elements of phosphorus and halogen simultaneously, has intramolecular synergistic effect, thus can be used alone, and general types are such as
Trichloro ethylene (TECP) etc..(3) nitrogen system.Principal item has trimerization nitrogen ammonia etc., is usually used in PA and PU, and assists with phosphorus type flame retardant
With use.Inorganic anti-flaming material general types have following several: (1) antimony oxide.Must cooperate with organic fire-resisting material makes
With.(2) magnesium hydroxide, aluminium hydroxide.It can use individually, but additional amount is big, it is often suitable with amount of resin.(3) inorganic
It is Phosphorus.Common red phosphorus and sulfate, pure red phosphorus is preceding last by treatment with micron in use, can be applied alone and be used in combination, phosphate has phosphorus
Sour ammonium, ammonium nitrate etc..(4) boron class fire proofing.Common hydration zinc borate, generally cooperates with use with other fire proofings.Other
Metal oxide, such as metal aluminide, metal iron compound, are mainly used for the smoke of gunpowder.(5) metal halide.Such as all kinds of antimony halides
Class.
Thus, it is also very desirable to by the improvement of formula, to obtain a novel black feed composition for building.
Summary of the invention
In order to solve the above-mentioned technical problem, the first aspect of the invention provides a kind of black feed composition for building, institute
Black feed composition for building is stated, in parts by weight, includes at least following components:
As a preferred technical solution of the present invention, the black feed composition for building includes at least in parts by weight
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 graphene is selected from: graphene oxide, sulfonated graphene, carboxylic
Base graphite alkene, amination graphene, any one or a few the mixing in graphene nanometer sheet.
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 black feed composition for building, includes at least following step
It is rapid:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
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 black feed composition for building, institute
Black feed composition for building is stated, in parts by weight, includes at least following components:
As a preferred technical solution of the present invention, the black feed composition for building includes at least in parts by weight
Following components:
As a preferred technical solution of the present invention, the black feed composition for building includes at least in parts by weight
Following components:
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.
Graphene
The two dimension for there was only one layer of atomic thickness that term " graphene " is stripped out from graphite material, is made of carbon atom
Crystal.
In a preferred embodiment, the graphene is selected from: graphene oxide, sulfonated graphene, carboxyl fossil
Black alkene, amination graphene, any one or a few the mixing in graphene nanometer sheet.
In a kind of most preferred embodiment, the graphene is selected from: graphene oxide, amination graphene it is mixed
It closes；The graphene oxide, amination graphene weight ratio be 100:(3~12)；Most preferably, the graphene oxide,
The weight ratio of amination graphene is 100:3.
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 black feed composition for building, includes at least following step
It is rapid:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
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 black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 2:
The embodiment of the present invention 2 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 3:
The embodiment of the present invention 3 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 4:
The embodiment of the present invention 4 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 5:
The embodiment of the present invention 5 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 6:
The embodiment of the present invention 6 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 7:
The embodiment of the present invention 7 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 8:
The embodiment of the present invention 8 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is graphene oxide, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 9:
The embodiment of the present invention 9 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part 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 graphene is amination graphene, is purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Embodiment 10:
The embodiment of the present invention 10 provides a kind of black feed composition for building, the black feed composition for building, with weight
Part meter is measured, following components is included at least:
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 graphene is the mixture of graphene oxide, amination graphene；The graphene oxide, amino fossil
The weight ratio of black alkene is 100:3；
The graphene oxide, amination graphene are purchased from Nanjing Xian Feng Nono-material Science & Technology 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 black feed composition for building, at least includes the following steps:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder are weighed according to corresponding parts by weight and are filled out
Material, after mixing, obtains black feed composition for building.
Comparative example 1:
Comparative example 1 is with embodiment 10, the difference lies in that A-B-C is replaced with B.
Comparative example 2:
Comparative example 2 is with embodiment 10, the difference lies in that A-B-C is replaced with nano silica.
Comparative example 3:
Comparative example 3 is with embodiment 10, 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 10, the difference lies in that A-B-C is replaced with maleic anhydride modified polypropylene.
Comparative example 5:
Comparative example 5 is with embodiment 10, the difference lies in that A-B-C is replaced with polypropylene.
Comparative example 6:
Comparative example 6 is with embodiment 10, the difference lies in that A-B-C is replaced with maleic acid.
Comparative example 7:
Comparative example 7 is with embodiment 10, 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 10, the difference lies in that A-B-C is replaced with ammonium polyphosphate.
Comparative example 9:
Comparative example 9 is with embodiment 10, the difference lies in that expanded graphite and graphene to be replaced with to the poly- phosphorus of corresponding parts by weight
Sour ammonium.
Comparative example 10:
Comparative example 10 is with embodiment 10, the difference lies in that not including graphene in formula.
Comparative example 11:
Comparative example 11 is with embodiment 10, the difference lies in that not including graphite in formula.
Comparative example 12:
Comparative example 12 is with embodiment 10, the difference lies in that the weight ratio of graphene oxide and ammonification graphene is 3:100.
Comparative example 13:
Comparative example 13 is with embodiment 10, the difference lies in that the weight ratio of graphene oxide and sulfonated graphene is 100:3.
The product that Examples 1 to 10 and comparative example 1~13 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 black feed composition for building
Weight ratio is 10:1.It is coated on plastic strip respectively, carries out test flame retardant property, chalking resistance energy and weather resistance.
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.
3, weatherability is carried out by GB/T 3511-2008 standard.
1 chalk rating of table
The rating and corresponding phenomenon of 2 artificial weathering aging exposure test of table
| Grade | Phenomenon |
| 0 | It is unchanged |
| 1 | Perceptible slight change |
| 2 | Moderate variation |
| 3 | Significant change |
3 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 black feed composition for building, which is characterized in that the black feed composition for building at least wraps in parts by weight
Include following components:
2. black feed composition for building as described in claim 1, which is characterized in that the black feed composition for building, with weight
Part meter is measured, following components is included at least:
3. black feed composition for building as described in claim 1, which is characterized in that the calcium carbonate is nanometer calcium carbonate.
4. black feed composition for building as described in claim 1, which is characterized in that the graphite is expanded graphite.
5. black feed composition for building as claimed in claim 4, which is characterized in that the expanded graphite is composite material intercalation
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 and are selected from: appointing in maleic anhydride modified polypropylene, end carboxyl super branched polyester
It anticipates one kind.
6. black feed composition for building as claimed in claim 5, which is characterized in that the B is selected from: amino silicane coupling agent changes
Property nano silica；The A is selected from: maleic anhydride modified polypropylene；The C is selected from: end carboxyl super branched polyester.
7. black feed composition for building as described in claim 1, which is characterized in that the graphene is selected from: graphene oxide,
Sulfonated graphene, carboxylated graphene, amination graphene, in graphene nanometer sheet in any one or a few mixing.
8. black feed composition for building as described in claim 1, which is characterized in that the calcium sulphate retarder is selected from: citric acid,
It is one or more in sodium polyphosphate, borax.
9. black feed composition for building as described in claim 1, which is characterized in that the filler is selected from: nano silica,
Nano aluminium oxide, talcum powder, montmorillonite, calcium oxide, wollastonite, any one or a few the mixing in mica.
10. the preparation method of the black feed composition for building as described in claim 1~9, which is characterized in that include at least following
Step:
Calcium carbonate, graphite, graphene, alpha-olefin sodium sulfonate, calcium sulphate retarder and filler are weighed according to corresponding parts by weight, is mixed
After closing uniformly, black feed composition for building is obtained.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2763063C1 (en) * | 2020-08-12 | 2021-12-27 | Общество с ограниченной ответственностью "ТЕХНОХИМ" | Functional filler for a fire extinguishing powder composition |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2763063C1 (en) * | 2020-08-12 | 2021-12-27 | Общество с ограниченной ответственностью "ТЕХНОХИМ" | Functional filler for a fire extinguishing powder composition |
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Application publication date: 20191015 |