CN107641468A - A kind of water proof fire retardant powdery paints and preparation method thereof - Google Patents
A kind of water proof fire retardant powdery paints and preparation method thereof Download PDFInfo
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- CN107641468A CN107641468A CN201711016174.7A CN201711016174A CN107641468A CN 107641468 A CN107641468 A CN 107641468A CN 201711016174 A CN201711016174 A CN 201711016174A CN 107641468 A CN107641468 A CN 107641468A
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Abstract
The present invention relates to technical field of chemical paint, discloses a kind of water proof fire retardant powdery paints and preparation method thereof.The raw material that the powdery paints is matched by following parts by weight is made：60 ~ 65 parts of modified propylene acid butyl ester resin, 20 ~ 30 parts of hollow glass micropearl, 2 ~ 6 parts of dodecanedioic acid, 2 ~ 4 parts of styrax, 1 ~ 3 part of catechol, 3 ~ 5 parts of polyacrylate, 2; 6 ~ 9 parts of 4,6 2 ~ 5 parts of trimethylbenzoyl phenyl etherophosphoric acids and modified magnesium hydroxide.First each component is well mixed in powdery paints preparation process, is then fed into screw extruder and carries out melting extrusion, crushes, place into pulverizer and crushed to obtain powdery paints.Powdery paints of the present invention has preferable water proof fire retardant effect.
Description
Technical field
The present invention relates to technical field of chemical paint, more particularly, to a kind of preferable coating of water proof fire retardant effect and its system
Preparation Method.
Background technology
Powdery paints is a kind of 100% solid powder without organic solvent, and it is different from oil paint and water paint,
Not using water as decentralized medium during application, but using air as decentralized medium, uniformly coated in workpiece surface, by heating
A kind of one layer of new type environment friendly coating with the coating of specific use is formed afterwards.Powdery paints has VOC free, environmental protection, saves, applies
The advantages that work efficiency high and wide application.Most of powdery paints easily come off after water is met from body surface in the market
And do not have flame retardant effect.
The content of the invention
The present invention is to overcome prior art powdery paints water proof fire retardant effect difference problem, there is provided one kind has preferably anti-
The powdery paints of water and flame retardant effect.
Present invention also offers a kind of preparation method of water proof fire retardant powdery paints.
To achieve these goals, the present invention uses following technical scheme：A kind of water proof fire retardant powdery paints, by following heavy
The raw material of amount number proportioning is made：60~65 parts of modified propylene acid butyl ester resin, 20~30 parts of hollow glass micropearl, dodecane two
2~6 parts of acid, 2~4 parts of styrax, 1~3 part of catechol, 3~5 parts of polyacrylate, 2,4,6- trimethylbenzoyl phenyls
6~9 parts of 2~5 parts of etherophosphoric acid and modified magnesium hydroxide.
The present invention is using modified propylene acid butyl ester resin as main component, and hollow glass micropearl is filler, and dodecanedioic acid is
Curing agent, styrax are degasser, catechol is antioxidant, polyacrylate is levelling agent, 2,4,6- trimethylbenzoyls
Phosphenylic acid ethyl ester is light trigger, modified magnesium hydroxide is fire retardant, and the powdery paints of preparation has preferable anti-aging, prevented
Ultraviolet and water proof fire retardant effect.
Preferably, the preparation method of the modified propylene acid butyl ester resin comprises the following steps：
(1) chlorohexanes of 160~180mL tetra- are added in four-hole bottle, then add 0.04~0.08mol tert-butyl hydroperoxides
Hydrogen, the air poured into four-hole bottle in nitrogen discharge four-hole bottle, oil bath heating add 0.45~0.6mol to 55~60 DEG C
Butyl acrylate, stirring reaction 2~3 hours, obtains butyl acrylate resin prepolymer；
(2) 2~3mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 4~5, is warming up to
55~65 DEG C, 0.03~0.06mol cumyl peroxides and 0.4~0.5mol dodecafluoroheptyl methacrylates are added, is stirred
Mix 50~60min of reaction；
(3) 0.3~0.5mol phenyl methyl silicone oils are added into the reaction solution of step (2), 1~2h of stirring reaction, are modified
Butyl acrylate resin.
Radical polymerization is first passed through, butyl acrylate resin prepolymer is prepared using butyl acrylate, then will prepare third
Olefin(e) acid butyl ester resin prepolymer and the further cross-linked polymeric of dodecafluoroheptyl methacrylate, make butyl acrylate resin macromolecular
In draw such as C-F keys, because C-F keys have stronger hydrophobic ability, so, introduce the butyl acrylate resin of C-F keys have compared with
Good hydrophobic ability；Graft reaction is occurred into for the butyl acrylate resin containing C-F keys and phenyl methyl silicone oil again, formation gathers
Compound has relatively low surface energy, further increases the hydrophobic performance of powdery paints, in addition, butyl acrylate resin is introduced
The higher group of the energy such as phenyl ring, enhance the heat resistance of powdery paints.
Wherein, the preparation method of the modified magnesium hydroxide comprises the following steps：
(1) magnesium hydrate powder is put into the vacuum drying oven that temperature is 70~80 DEG C and 4~8h is dried；
Processing is dried to magnesium hydroxide powder, prevents the moisture in subsequent reactions in magnesium hydroxide from being influenceed to caused by reaction.
(2) the tetrachloro hexane solution of completing to add 2~3 times of magnesium hydroxide weight in backward conical flask and dried is dried
Magnesium hydrate powder, the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 6~10% is then added, carry out magnetic force and stir
Mix, 1~2h of heating response；
Processing is alkylated to magnesium hydroxide using ethylenediaminepropyltriethoxysilane, magnesium hydroxide surface is incidentally had
The group that can be reacted with organic substance.
(3) Ractopamine, the magnesium hydroxide weight of magnesium hydroxide weight 5~8% are added into the reaction solution of step (2)
0.06~0.08% potassium peroxydisulfate and the carboxyl chitosan of magnesium hydroxide weight 6~12%, 3~4h of heating response；
Ractopamine has higher activity, and the magnesium hydroxide with being alkylated treated crosslinks reaction, makes magnesium hydroxide
Between attraction decline, reduce magnesium hydroxide between attraction, magnesium hydroxide is uniformly blended in component, improve it
Fire resistance；Carboxyl chitosan and the Ractopamine on magnesium hydroxide surface crosslink, and magnesium hydroxide surface is covered one layer
Carboxyl chitosan, so as to further improve the dispersive property of magnesium hydroxide；In addition, carboxyl chitosan has more reactive group
Group, such as amino, carboxyl, hydroxyl, it can crosslink reaction with other components in powdery paints, be favorably improved coating
Fire resistance；Magnesium hydroxide is by modified, and one layer of chitosan of its outer cladding, when running into external force, clad is to high polymer and hydrogen
Stress transmission is formed between aluminum oxide, the toughness of coating is improved by absorbing external force, prevents coating from holding under the shock of external force
Easily fall off.
(4) material that step (3) obtains is put into vacuum drying chamber and dries 4~6h, obtain modified magnesium hydroxide.
Preferably, heating-up temperature is 55~65 DEG C in the step (2).
Preferably, heating-up temperature is 70~85 DEG C in the step (3).
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Preferably, each area's temperature of screw extruder is respectively in the step (B)：One area's temperature：125~130 DEG C,
Two 140~150 DEG C of area's temperature, three 155~180 DEG C of area's temperature.
Therefore, the present invention has the advantages that：(1) the butyl acrylate resin tool for introducing C-F keys is preferably hydrophobic
Ability；(2) with phenyl methyl silicone oil graft reaction occurs for butyl acrylate resin, and the polymer of formation has relatively low surface
Energy, further increase the hydrophobic performance of powdery paints；(3) butyl acrylate resin has introduced the higher base of the energy such as phenyl ring
Group, enhance the heat resistance of powdery paints；(4) Ractopamine has higher activity, and it is with being alkylated treated hydrogen
Magnesia crosslinks reaction, declines the attraction between magnesium hydroxide, reduces the attraction between magnesium hydroxide, makes hydrogen-oxygen
Change magnesium to be uniformly blended in component, improve its fire resistance；(5) carboxyl chitosan has more reactive group, as amino,
Carboxyl, hydroxyl etc., it can crosslink reaction with other components in powdery paints, be favorably improved the fire resistance of coating；
(6) magnesium hydroxide is by modified, and one layer of chitosan of its outer cladding, when running into external force, clad is to high polymer and aluminium hydroxide
Between formed stress transmission, improve the toughness of coating by absorbing external force, prevent coating from easily occurring under the shock of external force
Come off.
Embodiment
Below by specific embodiment, technical scheme is described further.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art,
Method in embodiment, it is the conventional method of this area unless otherwise instructed.
Embodiment 1
A kind of water proof fire retardant powdery paints, the raw material matched by following parts by weight are made：60 parts of modified propylene acid butyl ester resin,
20 parts of hollow glass micropearl, 2 parts of dodecanedioic acid, 2 parts of styrax, 1 part of catechol, 3 parts of polyacrylate, 2,4,6- trimethyls
6 parts of 2 parts of benzoylphenyl etherophosphoric acid and modified magnesium hydroxide.
Wherein, the preparation method of the modified propylene acid butyl ester resin comprises the following steps：
(1) chlorohexanes of 160mL tetra- are added in four-hole bottle, 0.04mol TBHPs are then added, into four-hole bottle
The air poured in nitrogen discharge four-hole bottle, oil bath heating add 0.45mol butyl acrylates to 55 DEG C, and stirring reaction 2 is small
When, obtain butyl acrylate resin prepolymer；
(2) 2mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 4, is warming up to 55 DEG C, adds
Enter 0.03mol cumyl peroxides and 0.4mol dodecafluoroheptyl methacrylates, stirring reaction 50min；
(3) 0.3mol phenyl methyl silicone oils are added into the reaction solution of step (2), stirring reaction 1h, obtain modified acroleic acid fourth
Ester resin.
Wherein, the preparation method of the modified magnesium hydroxide comprises the following steps：
(1) magnesium hydrate powder is put into the vacuum drying oven that temperature is 70 DEG C and 4h is dried；
(2) dry and complete the tetrachloro hexane solution of 2 times of magnesium hydroxide weight of addition and dried hydroxide in backward conical flask
Magnesium powder body, the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 6% is then added, carry out magnetic agitation, be heated to 55
DEG C, react 1h；
(3) Ractopamine, the magnesium hydroxide weight 0.06% of magnesium hydroxide weight 5% are added into the reaction solution of step (2)
Potassium peroxydisulfate and magnesium hydroxide weight 6% carboxyl chitosan, be heated to 70 DEG C, react 3h；
(4) material that step (3) obtains is put into vacuum drying chamber and dries 4h, obtain modified magnesium hydroxide.
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes, screw extruder
Each area's temperature is respectively：One area's temperature：125 DEG C, two 140 DEG C of area's temperature, three 155 DEG C of area's temperature；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Embodiment 2
A kind of water proof fire retardant powdery paints, the raw material matched by following parts by weight are made：62 parts of modified propylene acid butyl ester resin,
22 parts of hollow glass micropearl, 3 parts of dodecanedioic acid, 2 parts of styrax, 1 part of catechol, 3 parts of polyacrylate, 2,4,6- trimethyls
7 parts of 3 parts of benzoylphenyl etherophosphoric acid and modified magnesium hydroxide.
Wherein, the preparation method of the modified propylene acid butyl ester resin comprises the following steps：
(1) chlorohexanes of 165mL tetra- are added in four-hole bottle, 0.05mol TBHPs are then added, into four-hole bottle
The air poured in nitrogen discharge four-hole bottle, oil bath heating add 0.5mol butyl acrylates, stirring reaction 2.2 to 56 DEG C
Hour, obtain butyl acrylate resin prepolymer；
(2) 2.2mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 4.2, is warming up to 58
DEG C, add 0.04mol cumyl peroxides and 0.42mol dodecafluoroheptyl methacrylates, stirring reaction 52min；
(3) 0.35mol phenyl methyl silicone oils are added into the reaction solution of step (2), stirring reaction 1.2h, obtain modified acroleic acid
Butyl ester resin.
Wherein, the preparation method of the modified magnesium hydroxide comprises the following steps：
(1) magnesium hydrate powder is put into the vacuum drying oven that temperature is 72 DEG C and 5h is dried；
(2) dry and complete the tetrachloro hexane solution of 2.2 times of magnesium hydroxide weight of addition and dried hydrogen-oxygen in backward conical flask
Change magnesium powder body, then add the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 7%, carry out magnetic agitation, be heated to
58 DEG C, react 1.2h；
(3) Ractopamine, the magnesium hydroxide weight 0.06% of magnesium hydroxide weight 6% are added into the reaction solution of step (2)
Potassium peroxydisulfate and magnesium hydroxide weight 8% carboxyl chitosan, be heated to 75 DEG C, react 3.2h；
(4) material that step (3) obtains is put into vacuum drying chamber and dries 4.5h, obtain modified magnesium hydroxide.
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes, screw extruder
Each area's temperature is respectively：One area's temperature：126 DEG C, two 142 DEG C of area's temperature, three 160 DEG C of area's temperature；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Embodiment 3
A kind of water proof fire retardant powdery paints, the raw material matched by following parts by weight are made：63 parts of modified propylene acid butyl ester resin,
25 parts of hollow glass micropearl, 4 parts of dodecanedioic acid, 3 parts of styrax, 2 parts of catechol, 4 parts of polyacrylate, 2,4,6- trimethyls
7.5 parts of 3.5 parts of benzoylphenyl etherophosphoric acid and modified magnesium hydroxide.
Wherein, the preparation method of the modified propylene acid butyl ester resin comprises the following steps：
(1) chlorohexanes of 170mL tetra- are added in four-hole bottle, 0.06mol TBHPs are then added, into four-hole bottle
The air poured in nitrogen discharge four-hole bottle, oil bath heating add 0.52mol butyl acrylates, stirring reaction 2.5 to 57 DEG C
Hour, obtain butyl acrylate resin prepolymer；
(2) 2.6mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 4.5, is warming up to 60
DEG C, add 0.045mol cumyl peroxides and 0.45mol dodecafluoroheptyl methacrylates, stirring reaction 55min；
(3) 0.4mol phenyl methyl silicone oils are added into the reaction solution of step (2), stirring reaction 1.6h, obtain modified acroleic acid
Butyl ester resin.
Wherein, the preparation method of the modified magnesium hydroxide comprises the following steps：
(1) magnesium hydrate powder is put into the vacuum drying oven that temperature is 76 DEG C and 6h is dried；
(2) dry and complete the tetrachloro hexane solution of 2.6 times of magnesium hydroxide weight of addition and dried hydrogen-oxygen in backward conical flask
Change magnesium powder body, then add the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 8%, carry out magnetic agitation, be heated to
60 DEG C, react 1.6h；
(3) Ractopamine, the magnesium hydroxide weight of magnesium hydroxide weight 6.5% are added into the reaction solution of step (2)
0.07% potassium peroxydisulfate and the carboxyl chitosan of magnesium hydroxide weight 9%, 78 DEG C are heated to, react 3.6h；
(4) material that step (3) obtains is put into vacuum drying chamber and dries 5h, obtain modified magnesium hydroxide.
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes, screw extruder
Each area's temperature is respectively：One area's temperature：127 DEG C, two 146 DEG C of area's temperature, three 170 DEG C of area's temperature；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Embodiment 4
A kind of water proof fire retardant powdery paints, the raw material matched by following parts by weight are made：64 parts of modified propylene acid butyl ester resin,
28 parts of hollow glass micropearl, 5 parts of dodecanedioic acid, 4 parts of styrax, 3 parts of catechol, 5 parts of polyacrylate, 2,4,6- trimethyls
8 parts of 4 parts of benzoylphenyl etherophosphoric acid and modified magnesium hydroxide.
Wherein, the preparation method of the modified propylene acid butyl ester resin comprises the following steps：
(1) chlorohexanes of 175mL tetra- are added in four-hole bottle, 0.07mol TBHPs are then added, into four-hole bottle
The air poured in nitrogen discharge four-hole bottle, oil bath heating add 0.55mol butyl acrylates, stirring reaction 2.8 to 58 DEG C
Hour, obtain butyl acrylate resin prepolymer；
(2) 2.8mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 4.8, is warming up to 62
DEG C, add 0.05mol cumyl peroxides and 0.48mol dodecafluoroheptyl methacrylates, stirring reaction 58min；
(3) 0.45mol phenyl methyl silicone oils are added into the reaction solution of step (2), stirring reaction 1.8h, obtain modified acroleic acid
Butyl ester resin.
Wherein, the preparation method of the modified magnesium hydroxide comprises the following steps：
(1) magnesium hydrate powder is put into the vacuum drying oven that temperature is 78 DEG C and 7h is dried；
(2) dry and complete the tetrachloro hexane solution of 2.8 times of magnesium hydroxide weight of addition and dried hydrogen-oxygen in backward conical flask
Change magnesium powder body, then add the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 9%, carry out magnetic agitation, be heated to
62 DEG C, react 1.8h；
(3) Ractopamine, the magnesium hydroxide weight 0.08% of magnesium hydroxide weight 7% are added into the reaction solution of step (2)
Potassium peroxydisulfate and magnesium hydroxide weight 8~10% carboxyl chitosan, be heated to 80 DEG C, react 3.8h；
(4) material that step (3) obtains is put into vacuum drying chamber and dries 5.5h, obtain modified magnesium hydroxide.
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes, screw extruder
Each area's temperature is respectively：One area's temperature：128 DEG C, two 148 DEG C of area's temperature, three 175 DEG C of area's temperature；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Embodiment 5
A kind of water proof fire retardant powdery paints, the raw material matched by following parts by weight are made：65 parts of modified propylene acid butyl ester resin,
30 parts of hollow glass micropearl, 6 parts of dodecanedioic acid, 4 parts of styrax, 3 parts of catechol, 5 parts of polyacrylate, 2,4,6- trimethyls
9 parts of 5 parts of benzoylphenyl etherophosphoric acid and modified magnesium hydroxide.
Wherein, the preparation method of the modified propylene acid butyl ester resin comprises the following steps：
(1) chlorohexanes of 180mL tetra- are added in four-hole bottle, 0.08mol TBHPs are then added, into four-hole bottle
The air poured in nitrogen discharge four-hole bottle, oil bath heating add 0.6mol butyl acrylates to 60 DEG C, and stirring reaction 3 is small
When, obtain butyl acrylate resin prepolymer；
(2) 3mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 5, is warming up to 65 DEG C, adds
Enter 0.06mol cumyl peroxides and 0.5mol dodecafluoroheptyl methacrylates, stirring reaction 60min；
(3) 0.5mol phenyl methyl silicone oils are added into the reaction solution of step (2), stirring reaction 2h, obtain modified acroleic acid fourth
Ester resin.
Wherein, the preparation method of the modified magnesium hydroxide comprises the following steps：
(1) magnesium hydrate powder is put into the vacuum drying oven that temperature is 80 DEG C and 8h is dried；
(2) dry and complete the tetrachloro hexane solution of 3 times of magnesium hydroxide weight of addition and dried hydroxide in backward conical flask
Magnesium powder body, the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 10% is then added, carry out magnetic agitation, be heated to 65
DEG C, react 2h；
(3) Ractopamine, the magnesium hydroxide weight 0.08% of magnesium hydroxide weight 8% are added into the reaction solution of step (2)
Potassium peroxydisulfate and magnesium hydroxide weight 12% carboxyl chitosan, be heated to 85 DEG C, react 4h；
(4) material that step (3) obtains is put into vacuum drying chamber and dries 6h, obtain modified magnesium hydroxide.
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes, screw extruder
Each area's temperature is respectively：One area's temperature：130 DEG C, two 150 DEG C of area's temperature, three 180 DEG C of area's temperature；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Comparative example 1
A kind of water proof fire retardant powdery paints, the raw material matched by following parts by weight are made：It is 63 parts of butyl acrylate resin, hollow
25 parts of glass microballoon, 4 parts of dodecanedioic acid, 3 parts of styrax, 2 parts of catechol, 4 parts of polyacrylate, 2,4,6- trimethylbenzene first
7.5 parts of 3.5 parts of aminosulfonylphenyl etherophosphoric acid and magnesium hydroxide.
A kind of preparation method of water proof fire retardant powdery paints, comprises the following steps：
(A) by the butyl acrylate resin of formulation weight part, hollow glass micropearl, dodecanedioic acid, styrax, catechol, poly-
Acrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and magnesium hydroxide, which are added in batch mixer, to be sufficiently mixed
It is even；
(B) batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes, screw extruder
Each area's temperature is respectively：One area's temperature：127 DEG C, two 146 DEG C of area's temperature, three 170 DEG C of area's temperature；
(C) material in step (B) is sent into pulverizer and crushed, obtain powdery paints.
Embodiment 1 is to embodiment 5, comparative example 1 (butyl acrylate resin and magnesium hydroxide are without by being modified) powder
The contact angle of coating such as following table：
The standby powdery paints of butyl acrylate resin-made after being modified by experimental result, hydrophobic performance obtain significantly
Improve, magnesium hydroxide passes through the modified fire resistance for considerably increasing powdery paints.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the technical spirit pair according to the present invention without departing from technical solution of the present invention content
Any simple modification, equivalent change and modification that above example is made, in the range of still falling within technical solution of the present invention.
Claims (7)
1. a kind of water proof fire retardant powdery paints, it is characterized in that, the raw material matched by following parts by weight is made：Modified acroleic acid fourth
It is 60 ~ 65 parts of ester resin, 20 ~ 30 parts of hollow glass micropearl, 2 ~ 6 parts of dodecanedioic acid, 2 ~ 4 parts of styrax, 1 ~ 3 part of catechol, poly-
6 ~ 9 parts of 3 ~ 5 parts of acrylate, 2 ~ 5 parts of 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide.
2. a kind of water proof fire retardant powdery paints according to claim 1, it is characterized in that, the modified propylene acid butyl ester resin
Preparation method comprise the following steps：
（1）The chlorohexanes of 160 ~ 180mL tetra- are added in four-hole bottle, then add 0.04 ~ 0.08mol TBHPs,
The air poured into four-hole bottle in nitrogen discharge four-hole bottle, oil bath heating add 0.45 ~ 0.6mol propylene to 55 ~ 60 DEG C
Acid butyl ester, stirring reaction 2 ~ 3 hours, obtains butyl acrylate resin prepolymer；
（2）2 ~ 3mol/L watery hydrochloric acid is added in butyl acrylate resin prepolymer liquid solution, regulation pH is 4 ~ 5, it is warming up to 55 ~
65 DEG C, add 0.03 ~ 0.06mol cumyl peroxides and 0.4 ~ 0.5mol dodecafluoroheptyl methacrylates, stirring reaction
50~60min；
（3）To step（2）Reaction solution in add 0.3 ~ 0.5mol phenyl methyl silicone oils, 1 ~ 2h of stirring reaction, obtain modified third
Olefin(e) acid butyl ester resin.
3. a kind of water proof fire retardant powdery paints according to claim 1, it is characterized in that, the preparation of the modified magnesium hydroxide
Method comprises the following steps：
（1）Magnesium hydrate powder is put into the vacuum drying oven that temperature is 70 ~ 80 DEG C 4 ~ 8h is dried；
（2）Dry and complete the tetrachloro hexane solution of 2 ~ 3 times of magnesium hydroxide weight of addition and dried hydrogen-oxygen in backward conical flask
Change magnesium powder body, then add the ethylenediaminepropyltriethoxysilane of magnesium hydroxide weight 6 ~ 10%, carry out magnetic agitation, heating
React 1 ~ 2h；
（3）To step（2）Reaction solution in add the Ractopamine of magnesium hydroxide weight 5 ~ 8%, magnesium hydroxide weight 0.06 ~
0.08% potassium peroxydisulfate and the carboxyl chitosan of magnesium hydroxide weight 6 ~ 12%, 3 ~ 4h of heating response；
（4）By step（3）Obtained material, which is put into vacuum drying chamber, dries 4 ~ 6h, obtains modified magnesium hydroxide.
4. a kind of water proof fire retardant powdery paints according to claim 3, it is characterized in that, the step（2）Middle heating-up temperature
For 55 ~ 65 DEG C.
5. a kind of water proof fire retardant powdery paints according to claim 3, it is characterized in that, the step（3）Middle heating-up temperature
For 70 ~ 85 DEG C.
6. a kind of preparation method of water proof fire retardant powdery paints as described in claim 1 ~ 5 any claim, it is characterized in that,
Comprise the following steps：
（A）By the modified propylene acid butyl ester resin, hollow glass micropearl, dodecanedioic acid, styrax, catechu of formulation weight part
Phenol, polyacrylate, 2,4,6- trimethylbenzoyl phenyls etherophosphoric acid and modified magnesium hydroxide are added in batch mixer and filled
Divide well mixed；
（B）Batch mixing after being well mixed, which is added in screw extruder, to carry out melting extrusion, tabletting, crushes；
（C）By step（B）In material be sent into pulverizer in crushed, obtain powdery paints.
7. a kind of preparation method of water proof fire retardant powdery paints according to claim 6, it is characterized in that, the step（B）
Each area's temperature of middle screw extruder is respectively：One area's temperature：125 ~ 130 DEG C, two 140 ~ 150 DEG C of area's temperature, three area's temperature 155
~180℃。
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| CN109553978A (en) * | 2018-11-23 | 2019-04-02 | 唐山师范学院 | Retarding chamber temperature vulcanizable silicone rubber compounding and fire-retardant room temperature vulcanized silicone rubber |
| CN111378299A (en) * | 2020-04-01 | 2020-07-07 | 辽宁精华新材料股份有限公司 | Method for modifying surface of magnesium hydroxide by using dopamine-induced transition metal ions |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109553978A (en) * | 2018-11-23 | 2019-04-02 | 唐山师范学院 | Retarding chamber temperature vulcanizable silicone rubber compounding and fire-retardant room temperature vulcanized silicone rubber |
| CN109553978B (en) * | 2018-11-23 | 2021-05-25 | 唐山师范学院 | Formula of flame-retardant room-temperature vulcanized silicone rubber and flame-retardant room-temperature vulcanized silicone rubber |
| CN111378299A (en) * | 2020-04-01 | 2020-07-07 | 辽宁精华新材料股份有限公司 | Method for modifying surface of magnesium hydroxide by using dopamine-induced transition metal ions |
| CN111378299B (en) * | 2020-04-01 | 2021-04-30 | 辽宁精华新材料股份有限公司 | Method for modifying surface of magnesium hydroxide by using dopamine-induced transition metal ions |
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