A kind of low cigarette environment-friendly fireproof coating and preparation method thereof
Technical field
The present invention relates to building product fields more particularly to a kind of low cigarette environment-friendly fireproof coating and preparation method thereof.
Background technique
With the continuous increase of Chinese national economy, various industries especially building trade often will appear fire incident,
Cause important casualties and property loss, trace it to its cause be primarily due to they used in process of construction it is many easily
The substance and material of combustion, and a large amount of smog and toxic gas are generated in combustion, these materials are investigated according to relevant departments
All without passing through various flame retardant treatments, great injury and injures and deaths are just caused.
According to related news, the fire that our various regions occur can be found everywhere, and also constantly increase, according to statistics the whole nation in 1999
Fire 39571 occurs to rise, death about 2652 people, about 5977 people of wound, about 11.2 hundred million yuan of direct economic loss;And fire in 2000
Calamity is about 40000, extremely about 2800 people, injury about 4000 people, and about 1,200,000,000 yuan of direct economic loss.In consideration of it, country is related
Department and expert call everybody to use nonflammable material in process of construction as far as possible, and to reach national requirements
Fire-protection rating, for example as the insulating layer of building envelopes has to reach corresponding fire-protection rating, could preferably reach in this way
Flameproof effect.The generation of fire incident in order to prevent, implements fire-fighting work conscientiously, fulfils the work of " putting prevention first, combine prevention with fire fighting "
Make policy, country has formulated corresponding laws and regulations, calls using fireproof coating and fire proofing to prevent fire, therefore
Fireproofing becomes more and more important, more more and more urgent.From the point of view of us now used construction material, most of ratios are easier to
Combustion, there are many violations of rules and regulations, substantially also without just directly applying by corresponding fire prevention processing, and in combustion
There are no good fire prevention measure, masses' awareness of the importance of fire prevention is weaker, and many accidents is caused constantly to occur.In numerous fire prevention means
It is that can achieve preferable flameproof effect using fireproof coating that middle comparison is effectively and application is wider.
Traditional fireproof coating is mainly based upon macromolecule matrix, including propylene acid esters, epoxy resin, and esters of silicon acis etc. is organic
Resin.And their main application technology is spraying, is brushed, roller coating etc., another method is exactly that material surface is directly soaked
Stain in coating, make its infiltrate through in material achieve the effect that it is fire-retardant.However these technologies are there are problems, for example method
It is too cumbersome, furthermore a large amount of raw material and chemicals are needed, serious pollution, and duplicate brushing, meeting are caused to environment
Cause the adhesion strength between coating not strong, the problem of being easy to fall off.
Thus, it is also very desirable to a kind of effective study on formula of fireproof paint is developed, so that in fire generating process, effectively
Inhibit the sprawling of fire, while smoke creating amount can be significantly reduced, for reducing fire casualties, improves related places
Fire safety grade.
Summary of the invention
In order to solve the above-mentioned technical problem, the first aspect of the invention provides low cigarette environment-friendly fireproof coating, with weight
Part meter is measured, including at least following raw material: 30~50 parts of cement;12~25 parts of cellulose;12~30 parts of semi-hydrated gypsum;Calcium carbonate 1
~6 parts;5~10 parts of polystyrene board;1~3 part of graphene, 1~5 part of foaming agent;1~3 part of retarder.
As a preferred technical solution of the present invention, the cement is selected from: portland slag cement, volcano grey matter silicic acid
Salt cement, fine coal grey matter portland cement, magnesium phosphate cement, any one or a few the mixing in potassium magnesium phosphate cement.
As a preferred technical solution of the present invention, the cellulose is selected from: methylcellulose, hydroxypropyl methyl fiber
Element, hydroxyethyl cellulose, carboxymethyl cellulose, flax fiber element, ramee element, tossa element, bamboo fibre, mineral are fine
Any one or a few mixing in dimension, glass fibre.
As a preferred technical solution of the present invention, the low cigarette environment-friendly fireproof coating further includes auxiliary agent, described to help
Agent is selected from: insulation agent, foaming agent, fire retardant, synergistic flame retardant, smoke inhibition fire retardant, smoke-inhibiting flame retardant synergist, ultraviolet radiation absorption
Agent, filler, any one or a few the mixing in talcum powder.
As a preferred technical solution of the present invention, the talcum powder is the microsphere modified talcum powder of aminopolystyrene.
As a preferred technical solution of the present invention, the filler is selected from: in expanded graphite particles, hollow glass micropearl
Any one or a few mixing.
As a preferred technical solution of the present invention, the smoke inhibition fire retardant are as follows: methylol ferrocene, ammonium polyphosphate change
The compound of property nanometer hydroxyapatite, graphene oxide;The methylol ferrocene, ammonium polyphosphate modified Nano hydroxy-apatite
Weight ratio between stone, graphene oxide are as follows: 3:10:1.
As a preferred technical solution of the present invention, the low cigarette environment-friendly fireproof coating further includes the super of 5 parts by weight
Branching polyphosphate resin.
As a preferred technical solution of the present invention, the low cigarette environment-friendly fireproof coating further includes 1~5 parts by weight
Modified mesoporous silicon oxide;The modified mesoporous silicon oxide the preparation method is as follows:
The hydroxy-end capped polyurethane resin of 5~20 parts by weight molten conditions and 1~5 parts by weight mesoporous silicon oxide are mixed
It closes, in the case where temperature is 150 DEG C, stirs 1~3h.
The second aspect of the invention provides a kind of preparation method of low cigarette environment-friendly fireproof coating, includes at least following
Step:
(1) cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent are existed by above-mentioned weight ratio
10~60min is stirred under 1000~1200 revs/min, is uniformly mixed;
(2) cellulose, the graphene that corresponding parts by weight are added into step (1) stir 20 under 2000~4000 revs/min
~60min develops fineness to 70~100um after mixing, disperses after stirring evenly to obtain the final product.
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 low cigarette environment-friendly fireproof coating, with weight
Part meter is measured, following raw material: cement 30~50 is included at least;Cellulose 12~25;Semi-hydrated gypsum 12~30;Calcium carbonate 1~6;It is poly-
Styrene plate 5~10;Graphene 1~3;Talcum powder 1~5;Nanometer hydroxyapatite 3~8;Filler 3~10;Auxiliary agent 3~10.
Cement
In the application, the cement is not particularly limited, and is commercially available acquisition.
In a preferred embodiment, the cement is selected from: portland slag cement, portland-pozzolana water
Mud, fine coal grey matter portland cement, magnesium phosphate cement, any one or a few the mixing in potassium magnesium phosphate cement.
Cellulose
In the application, the cellulose is not particularly limited, and is commercially available acquisition.
In a preferred embodiment, the cellulose is selected from: methylcellulose, hydroxypropyl methyl cellulose, hydroxyl
Ethyl cellulose, carboxymethyl cellulose, flax fiber element, ramee element, tossa element, bamboo fibre, mineral fibres, glass
Any one or a few mixing in fiber.
Semi-hydrated gypsum
In the application, the semi-hydrated gypsum is commercially available acquisition, is purchased from Zhengzhou sea-freight special cement Co., Ltd.
Calcium carbonate
In the application, " calcium carbonate " is nanometer calcium carbonate, and it is limited that the nanometer calcium carbonate is purchased from Changxing morning bright chemical industry
Company.
Polystyrene board
In the application, the polystyrene board is not particularly limited, and can be the poly- of commercially available any trade mark
Styrene plate.
In a preferred embodiment, the polystyrene board is sulfonated polystyrene microballoon.
In a preferred embodiment, the preparation method of the sulfonated polystyrene microballoon includes at least following step
It is rapid:
It takes 1g polystyrene microsphere that the 20g concentrated sulfuric acid is added, is 30 DEG C in temperature, is stirred to react 5 hours, is diluted with distilled water
The concentrated sulfuric acid is centrifuged and is dried in vacuo after repeatedly washing, obtains flaxen sulfonated polystyrene microballoon;
The polystyrene microsphere is purchased from big goose (Tianjin) Science and Technology Ltd..
Graphene
In the application, " graphene " is not particularly limited, and the graphene, which is purchased from Suzhou perseverance ball graphene, to be had
Limit company.
Talcum powder
In the application, " talcum powder " is not particularly limited, and can be the talcum of commercially available any trade mark
Powder.
In a preferred embodiment, the talcum powder is the microsphere modified talcum powder of aminopolystyrene.
In a preferred embodiment, the preparation method of the microsphere modified talcum powder of the aminopolystyrene include with
Lower step:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The aminopolystyrene microballoon is purchased from big goose (Tianjin) Science and Technology Ltd..
Nanometer hydroxyapatite
Nanometer hydroxyapatite in the present invention is not particularly limited, and is commercially available acquisition.
Hydroxyapatite, also known as hydroxyapatite, alkali calcium phosphate are apatite calcium (Ca5(PO4)3(OH)) natural mineral
Change.
Nanometer hydroxyapatite in the present invention is purchased from Xi'an Jin Heng Chemical Co., Ltd..
Filler
Filler in the application is not particularly limited.
In a preferred embodiment, the filler is selected from: any in expanded graphite particles, hollow glass micropearl
One or more of mixing.
Auxiliary agent
Auxiliary agent in the application is not particularly limited.
In a preferred embodiment, the auxiliary agent is selected from: insulation agent, foaming agent, fire retardant, synergistic flame retardant,
Smoke inhibition fire retardant, smoke-inhibiting flame retardant synergist, any one or a few the mixing in ultraviolet absorbing agent.
In a preferred embodiment, the smoke inhibition fire retardant are as follows: methylol ferrocene, ammonium polyphosphate modified Nano
The compound of hydroxyapatite, graphene oxide.
In a preferred embodiment, the methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, oxygen
In the compound of graphite alkene, methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, the weight between graphene oxide
Measure ratio are as follows: 3:10:1.
In a preferred embodiment, the ammonium polyphosphate modifted-nano-hydroxyapatite the preparation method is as follows:
(1) by 5g nanometer hydroxyapatite and 80mL SOC12Then mixing is added 150mL DMF as catalyst, hangs
Supernatant liquid is first crushed in crusher, and mixed solution is then placed in back flow reaction in 80 DEG C of oil baths, is filtered, after drying, is obtained acyl
Chlorinated hydroxyapatite;
(2) chloride hydroxyapatite obtained in step (1), 10g ammonium polyphosphate are mixed in 500mL DMF solvent
It closes, is placed in 85 DEG C of oil bath pans and reacts, ammonium polyphosphate modifted-nano-hydroxyapatite is finally obtained after filtering and drying.
In a preferred embodiment, the methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, oxygen
The compound of graphite alkene the preparation method is as follows:
It adds graphene oxide into the ethyl alcohol that mass fraction is 50%, strong stirring and 0.5~1h of ultrasonic disperse, so
It is added methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite at the same time afterwards, strong stirring and ultrasonic disperse 0.5~
1h is filtered under diminished pressure after cooling, and is washed with distilled water and dehydrated alcohol, and 50~80 DEG C of 10~12h of vacuum drying, ultra-fine grinding is extremely
More than 2000 mesh, obtain the compound of methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide.
What the fire retardant can be enumerated has: organophosphorus ester based flameproofing, Firemaster 836 based flameproofing, Phos base
Fire retardant, halogenated bisphenols based flameproofing, halogenated compound based flameproofing, antimony based flameproofing, nitrogen based flameproofing, boryl fire retardant,
Metal salt based flame retardants, inorganic fire retardants and silicon substrate fire retardant.These fire retardants can be used alone or in combination.
Organophosphorus ester or phosphite ester based flameproofing can be exemplified by, triphenyl phosphate, the new benzyl ester of phosphoric acid methyl, season penta
Tetrol diethyl bisphosphate, phosphoric acid methyl neopentyl ester, phosphoric acid phenyl neopentyl ester, pentaerythrite diphenyl bisphosphate,
Hypophosphoric acid bicyclopentyl ester, even diphosphorous acid di neo-pentyl ester, phenyl pyrocatechol phosphite ester, ethyl pyrocatechol phosphoric acid
Ester and two pyrocatechol hypophosphoric acid esters etc..
Firemaster 836 based flameproofing can be exemplified by, for example, tricresyl phosphate (β-chloroethyl) ester, tricresyl phosphate (Bicyclopropyl)
Ester, tricresyl phosphate (β-bromoethyl) ester, tricresyl phosphate (dibromopropyl) ester, tricresyl phosphate (chloropropyl) ester, tricresyl phosphate (dibromo phenyl) ester,
Tricresyl phosphate (tribromo phenyl) ester, tricresyl phosphate (tribromo neopentyl) ester, condensation polyphosphate and condensation polyphosphonates etc..
Inorganic phosphine flame retardant can be exemplified by, red phosphorus and inorganic phosphate.
Halogenated bisphenols based flameproofing can be exemplified by, tetrabromobisphenol A, its oligomer and two (bromoethyl ether) tetrabromobisphenol As.
Halogen compounds based flameproofing can be exemplified by decabrominated dipheny base ether, hexabromobenzene, hexabromocyclododecane, tetrabromo-phthalic two
Formic anhydride, (tetrabromobisphenol) epoxy oligomer, hexabromobiphenyl ether, tribromphenol, toluene tribromide base glycidol ether, decabrominated dipheny
Ether, halogenated polycarbonates, halogenated polycarbonates copolymer, halogenated polystyrene, halogenated polyolefin, chlorinated paraffin and the perchloro- ring last of the ten Heavenly stems
Alkane.
Antimony based flameproofing can be exemplified by, for example, antimony trioxide, four antimony oxides, antimony pentaoxide and antimonious acid sodium.
Nitrogen-based flameproofing can be exemplified by, for example, melamine, melamine that melamine, alkyl group replace or aromatic group replaces
Cyanurate, melamine isocyanurate, melamine phosphate, triazine, guanidine compound, urea, various cyanuric acid derivatives and phosphonitrile
(phosphasene) compound.
The example of boric acid based flameproofing may include zinc borate, zinc metaborate and barium metaborate.The example of metal salt based flame retardants
Attached bag includes the alkali metal salt and alkaline earth of perfluoroalkane sulfonate, alkyl benzene sulphonate, halogenated alkyl benzene sulfonic acid, alkyl sulfonic acid and naphthalene sulfonic acids
Metal salt.
Inorganic fire retardants can be exemplified by, magnesium hydroxide, aluminium hydroxide, barium hydroxide, calcium hydroxide, dolomite, hydrotalcite,
Basic magnesium carbonate, zircoium hydride, the hydrate (hydrate of such as tin oxide) of inorganic metal compound, metal oxide are (as aoxidized
Aluminium, iron oxide, titanium oxide, manganese oxide, magnesia, zirconium oxide, zinc oxide, molybdenum oxide, cobalt oxide, bismuth oxide, chromium oxide, oxidation
Tin, nickel oxide, copper oxide and tungsten oxide), metal (such as aluminium, iron, copper, nickel, titanium, manganese, tin, zinc, molybdenum, cobalt, bismuth, chromium, tungsten and antimony)
Powder and carbonate (such as zinc carbonate, magnesium carbonate, calcium carbonate and barium carbonate).
Ultraviolet absorbing agent can be exemplified by, 2- (2- hydroxy-5-methyl base phenyl) benzotriazole, 2- (2- hydroxyl -5- butyl benzene
Base) benzotriazole, 2- (2- hydroxyl -5- octyl phenyl) benzotriazole, 2- (3- tert-butyl -2- hydroxy-5-methyl base phenyl) -5- chlorine
Benzotriazole, 2- (3,5- bis- tertiary pentyl -2- hydroxy phenyl) benzotriazole, ESCALOL 567,2- hydroxyl -
4- n-octyl oxygroup benzophenone, 2- [4,6- bis- (2,4- 3,5-dimethylphenyl) -1,3,5-triazines -2- bases] -5- (octyl oxygroup)
Any one or a few mixing in phenol.
In a preferred embodiment, the gypsum base fireproof coating further includes the hyper branched polyphosphate of 5 parts by weight
Ester resin.
In a preferred embodiment, the gypsum base fireproof coating further includes the modification mesoporous two of 1~5 parts by weight
Silica;The modified mesoporous silicon oxide the preparation method is as follows:
The hydroxy-end capped polyurethane resin of 5~20 parts by weight molten conditions and 1~5 parts by weight mesoporous silicon oxide are mixed
It closes, in the case where temperature is 150 DEG C, stirs 1~3h.
The second aspect of the invention provides a kind of preparation method of low cigarette environment-friendly fireproof coating, includes at least following
Step:
(1) above-mentioned weight ratio is pressed by cement, semi-hydrated gypsum, calcium carbonate, talcum powder, polystyrene board, filler, auxiliary agent
10~60min is stirred under 1000~1200 revs/min, is uniformly mixed;
(2) to be added in step (1) celluloses of corresponding parts by weight, nanometer hydroxyapatite, modified mesoporous silicon oxide,
Hyper branched polyphosphate ester resin stirs 20~60min under 2000~4000 revs/min, develop after mixing fineness to 70~
100um disperses after stirring evenly to obtain the final product.
The applicant by a large amount of experimental studies have found that, after modified mesoporous silicon oxide is added, modified meso-porous titanium dioxide
Methylol ferrocene in silicon and smoke inhibition fire retardant can play the role of concerted catalysis, can be by the decomposition product or burning of substrate
Combustion product or smog are catalytically conveted to non-flammable compressive gas, to achieve the purpose that smoke-inhibiting flame retardant.
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 low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent are existed by above-mentioned weight ratio
10min is stirred under 1200 revs/min, is uniformly mixed;
(2) cellulose, the graphene that corresponding parts by weight are added into step (1) stir 20min under 4000 revs/min, mix
Fineness is developed after closing uniformly to 100um, is dispersed after stirring evenly to obtain the final product.
Embodiment 2:
The embodiment of the present invention 2 provides a kind of low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent are existed by above-mentioned weight ratio
10min is stirred under 1200 revs/min, is uniformly mixed;
(2) cellulose, the graphene that corresponding parts by weight are added into step (1) stir 20min under 4000 revs/min, mix
Fineness is developed after closing uniformly to 100um, is dispersed after stirring evenly to obtain the final product.
Embodiment 3:
The embodiment of the present invention 3 provides a kind of low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent are existed by above-mentioned weight ratio
10min is stirred under 1200 revs/min, is uniformly mixed;
(2) cellulose, the graphene that corresponding parts by weight are added into step (1) stir 20min under 4000 revs/min, mix
Fineness is developed after closing uniformly to 100um, is dispersed after stirring evenly to obtain the final product.
Embodiment 4:
The embodiment of the present invention 4 provides a kind of low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The talcum powder is the microsphere modified talcum powder of aminopolystyrene;
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) above-mentioned weight ratio is pressed by cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent, resistance
Combustion agent, smoke inhibition fire retardant stir 10min under 1200 revs/min, are uniformly mixed;
(2) cellulose, graphene, the talcum powder that corresponding parts by weight are added into step (1) stir under 4000 revs/min
20min develops fineness to 100um after mixing, disperses after stirring evenly to obtain the final product.
Embodiment 5:
The embodiment of the present invention 5 provides a kind of low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The talcum powder is the microsphere modified talcum powder of aminopolystyrene;
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The fire retardant is triphenyl phosphate;
The smoke inhibition fire retardant are as follows: methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide
Compound;The methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, the weight ratio between graphene oxide are as follows:
3:10:1.
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The preparation method of the smoke inhibition fire retardant the following steps are included:
(1) by 5g nanometer hydroxyapatite and 80mL SOC12Then mixing is added 150mL DMF as catalyst, hangs
Supernatant liquid is first crushed in crusher, and mixed solution is then placed in back flow reaction in 80 DEG C of oil baths, is filtered, after drying, is obtained acyl
Chlorinated hydroxyapatite;
(2) chloride hydroxyapatite obtained in step (1), 10g ammonium polyphosphate are mixed in 500mL DMF solvent
It closes, is placed in 85 DEG C of oil bath pans and reacts, ammonium polyphosphate modifted-nano-hydroxyapatite is finally obtained after filtering and drying.
(3) it adds graphene oxide into the ethyl alcohol that mass fraction is 50%, strong stirring and ultrasonic disperse 1h, then
Methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, strong stirring and ultrasonic disperse 1h are added at the same time, after cooling
It is filtered under diminished pressure, and is washed with distilled water and dehydrated alcohol, 80 DEG C of vacuum drying 12h, ultra-fine grinding obtains methylol to 2000 mesh
Ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide compound.
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) above-mentioned weight ratio is pressed by cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent, resistance
Combustion agent, smoke inhibition fire retardant stir 10min under 1200 revs/min, are uniformly mixed;
(2) cellulose, graphene, the talcum powder that corresponding parts by weight are added into step (1) stir under 4000 revs/min
20min develops fineness to 100um after mixing, disperses after stirring evenly to obtain the final product.
Embodiment 6:
The embodiment of the present invention 6 provides a kind of low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The talcum powder is the microsphere modified talcum powder of aminopolystyrene;
The hyper branched polyphosphate ester resin is purchased from Wuhan hyperbranched resin Co., Ltd.
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The fire retardant is triphenyl phosphate;
The smoke inhibition fire retardant are as follows: methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide
Compound;The methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, the weight ratio between graphene oxide are as follows:
3:10:1.
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The preparation method of the smoke inhibition fire retardant the following steps are included:
(1) by 5g nanometer hydroxyapatite and 80mL SOC12Then mixing is added 150mL DMF as catalyst, hangs
Supernatant liquid is first crushed in crusher, and mixed solution is then placed in back flow reaction in 80 DEG C of oil baths, is filtered, after drying, is obtained acyl
Chlorinated hydroxyapatite;
(2) chloride hydroxyapatite obtained in step (1), 10g ammonium polyphosphate are mixed in 500mL DMF solvent
It closes, is placed in 85 DEG C of oil bath pans and reacts, ammonium polyphosphate modifted-nano-hydroxyapatite is finally obtained after filtering and drying.
(3) it adds graphene oxide into the ethyl alcohol that mass fraction is 50%, strong stirring and ultrasonic disperse 1h, then
Methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, strong stirring and ultrasonic disperse 1h are added at the same time, after cooling
It is filtered under diminished pressure, and is washed with distilled water and dehydrated alcohol, 80 DEG C of vacuum drying 12h, ultra-fine grinding obtains methylol to 2000 mesh
Ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide compound.
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) above-mentioned weight ratio is pressed by cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent, resistance
Combustion agent, smoke inhibition fire retardant stir 10min under 1200 revs/min, are uniformly mixed;
(2) cellulose, graphene, talcum powder, the hyper branched polyphosphate ester resin of corresponding parts by weight are added into step (1)
It stirs 20min under 4000 revs/min, develops fineness after mixing to 100um, disperse after stirring evenly to obtain the final product.
Embodiment 7:
The embodiment of the present invention 7 provides a kind of low cigarette environment-friendly fireproof coating, in parts by weight, includes at least following original
Material:
The cement is portland cement, is purchased from China Resources cement Pty Ltd;
The cellulose is glass fibre, is purchased from Taishan glass fiber Ltd;
The semi-hydrated gypsum is purchased from Zhengzhou sea-freight special cement Co., Ltd
The calcium carbonate is nanometer calcium carbonate, is purchased from Changxing Chen Ming Chemical Co., Ltd.;;
The polystyrene board is purchased from big goose (Tianjin) Science and Technology Ltd.;
The graphene is purchased from Suzhou Heng Qiu graphene Co., Ltd;
The foaming agent is azodicarbonamide;
The retarder is calcium lignosulfonate;
The talcum powder is the microsphere modified talcum powder of aminopolystyrene;
The hyper branched polyphosphate ester resin is purchased from Wuhan hyperbranched resin Co., Ltd.
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The fire retardant is triphenyl phosphate;
The smoke inhibition fire retardant are as follows: methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide
Compound;The methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, the weight ratio between graphene oxide are as follows:
3:10:1.
The preparation method of the microsphere modified talcum powder of aminopolystyrene the following steps are included:
(1) by talcum powder in Muffle furnace in 300 DEG C progress constant temperature activating pretreatment about 3 hours, taking-up be down to room temperature, obtain
To treated talcum powder;
(2) talcum powder that will obtain that treated in step (1), 200ml phosphoric acid solution are mixed in planetary ball mill
Mechanical blending is carried out under the conditions of 150r/min, and mixed liquor is transferred to electric mixer, thermometer and reflux after twenty minutes
In the three-necked flask of condenser pipe, the reaction was continued under condition of water bath heating, when temperature is increased to 100 DEG C, by amino polyphenyl second
Alkene microballoon is added in three-necked flask, when to 200 DEG C, is stirred to react 2h, and sieve is crushed and crossed after being cooled to room temperature, is stored in drying
It is spare to obtain the microsphere modified talcum powder of aminopolystyrene in device.
The preparation method of the smoke inhibition fire retardant the following steps are included:
(1) by 5g nanometer hydroxyapatite and 80mL SOC12Then mixing is added 150mL DMF as catalyst, hangs
Supernatant liquid is first crushed in crusher, and mixed solution is then placed in back flow reaction in 80 DEG C of oil baths, is filtered, after drying, is obtained acyl
Chlorinated hydroxyapatite;
(2) chloride hydroxyapatite obtained in step (1), 10g ammonium polyphosphate are mixed in 500mL DMF solvent
It closes, is placed in 85 DEG C of oil bath pans and reacts, ammonium polyphosphate modifted-nano-hydroxyapatite is finally obtained after filtering and drying.
(3) it adds graphene oxide into the ethyl alcohol that mass fraction is 50%, strong stirring and ultrasonic disperse 1h, then
Methylol ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, strong stirring and ultrasonic disperse 1h are added at the same time, after cooling
It is filtered under diminished pressure, and is washed with distilled water and dehydrated alcohol, 80 DEG C of vacuum drying 12h, ultra-fine grinding obtains methylol to 2000 mesh
Ferrocene, ammonium polyphosphate modifted-nano-hydroxyapatite, graphene oxide compound.
Modified mesoporous silicon oxide the preparation method is as follows:
The hydroxy-end capped polyurethane resin of 5 parts by weight molten conditions and 1 parts by weight mesoporous silicon oxide are mixed, in temperature
Degree is to stir 1~3h at 150 DEG C;The hydroxy-end capped polyurethane resin is purchased from zero mound morning twilight resin Co., Ltd of Yongzhou City,
Product grade is TPU 6817;The mesoporous silicon oxide is purchased from Nanjing Ji Cang nanosecond science and technology Co., Ltd.
The preparation method of low cigarette environment-friendly fireproof coating, at least includes the following steps:
(1) above-mentioned weight ratio is pressed by cement, semi-hydrated gypsum, calcium carbonate, polystyrene board, retarder, foaming agent, resistance
Combustion agent, smoke inhibition fire retardant stir 10min under 1200 revs/min, are uniformly mixed;
(2) to be added in step (1) celluloses of corresponding parts by weight, graphene, talcum powder, modified mesoporous silicon oxide,
Hyper branched polyphosphate ester resin stirs 20min under 4000 revs/min, develops fineness after mixing to 100um, disperses after stirring evenly
To obtain the final product.
Comparative example 1:
Comparative example 1 of the invention is with embodiment 5, the difference lies in that the smoke inhibition fire retardant is commercially available zinc aluminate.
Comparative example 2:
Comparative example 2 of the invention is with embodiment 5, the difference lies in that the smoke inhibition fire retardant is methylol ferrocene.
Comparative example 3:
Comparative example 3 of the invention is with embodiment 5, the difference lies in that the smoke inhibition fire retardant is ammonium polyphosphate modified Nano
Hydroxyapatite.
Comparative example 4:
Comparative example 4 of the invention is with embodiment 5, the difference lies in that the smoke inhibition fire retardant is graphene oxide.
Comparative example 5:
Comparative example 5 of the invention is with embodiment 5, the difference lies in that the smoke inhibition fire retardant is ammonium polyphosphate.
The fireproof coating that all embodiments, comparative example obtain is applied to polyethylene surface, and for carrying out fire prevention experiment.
Performance evaluation
1, oxygen index (OI) test is carried out by ISO4589-1984, and batten is having a size of 130.0mm × 6.5mm × 3.0mm.
2, horizontal vertical burning is tested according to UL94 horizontal vertical combustion method.
3, smoke density test is carried out by ASTME662-95, batten size 40.0mm × 40.0mm × 3.0mm.
4, fire resistance period is referring to GB15442.2-1995.
1 characterization test of table
From table 1 it follows that Examples 1 to 7 and the low cigarette environment-friendly fireproof coating of comparative example 1~5 in the present invention
With extraordinary fire prevention, fire-retardant, smoke suppressing.
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.