CN110305512A - A kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic - Google Patents
A kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic Download PDFInfo
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- CN110305512A CN110305512A CN201910621608.9A CN201910621608A CN110305512A CN 110305512 A CN110305512 A CN 110305512A CN 201910621608 A CN201910621608 A CN 201910621608A CN 110305512 A CN110305512 A CN 110305512A
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- polyethylene glycol
- glycol monooleate
- halogen
- flame retardants
- antistatic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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Abstract
The present invention relates to halogen-free flame retardants preparation technical fields, and disclose a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic, including following tests raw material, polyethylene glycol monooleate, antioxidant compound, organic silicon flame-retardant adjuvant, collaboration metal-non-metal catalyst, the polyethylene glycol monooleate are the polymer of oleic acid and polyethylene glycol.The polyethylene glycol monooleate halogen-free flame retardants of the antistatic, cooperateing with metal-non-metal catalyst is the compound of bis cyclopentadienyl zirconium dichloride and N-bromosuccinimide, pass through bis cyclopentadienyl zirconium dichloride, by a small amount of polyethylene glycol monooleate by coordination at poly- glyoxal class monoleate compound, under the catalysis of N-chlorosuccinimide, poly- glyoxal class monoleate compound chlorination is poly- ethanedioly chloride monoleate, poly- ethanedioly chloride monoleate forms crosslinking band between polyethylene glycol monooleate polymer, make polyethylene glycol monooleate polymer that there is stable electric conductivity.
Description
Technical field
The present invention relates to halogen-free flame retardants preparation technical field, specially a kind of polyethylene glycol monooleate of antistatic without
Halogen fire retardant.
Background technique
The function of fire retardant is the functional aid for making combustible polymers have flame retardancy, primarily directed to high molecular material
Principle And Method of Flame Retardation Design, fire retardant mainly has inorganic fire retardants and organic fire-retardant at present, wherein mainly based on halogen flame,
But since halogenated flame retardant generates more cigarette and corrosive gas in thermal cracking or burning, environment is caused seriously to pollute,
The use of halogenated flame retardant has had become increasingly limited, and existing fire retardant does not have the work for making material antistatic
With.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, it the present invention provides a kind of cellulose base halogen-free flame retardants of insulating properties, solves
Existing fire retardant the problem of containing toxic halogen, while fire retardant does not have the problem of anti-static function.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme: a kind of polyethylene glycol monooleate of antistatic without
Halogen fire retardant, the raw material including following parts by weight proportion, it is characterised in that: 50-60 parts of polyethylene glycol monooleates, 0.3-
0.8 part of antioxidant compound, 40-50 parts of organic silicon flame-retardant adjuvants, 0.1-0.3 parts of collaboration metal-non-metal catalyst.
Preferably, the polyethylene glycol monooleate is the polymer of oleic acid and polyethylene glycol, and preparation method is as follows:
(1) 20g oleic acid and 50mL1 are weighed, 4- dioxane is sequentially placed into 500mL beaker, adds 35g polyethylene glycol
With 2g catalyst benzene sulfonic acid, then heating water bath is to 70 DEG C, at the uniform velocity stirring 12h；
(2) it after fully reacting, is cooled to room temperature, 5 sodium bicarbonates is added into the beaker of above-mentioned steps (1), at the uniform velocity stir
20-30min neutralizes benzene sulfonic acid；
(3) 40g polyethylene glycol is added to be extracted, vacuum distillation removes Isosorbide-5-Nitrae-dioxane after extraction, filters crude product
Obtain polyethylene glycol monooleate.
Preferably, the collaboration metal-non-metal catalyst is the compound of bis cyclopentadienyl zirconium dichloride and N-bromosuccinimide
Object, mass ratio 6:1.By bis cyclopentadienyl zirconium dichloride, by a small amount of polyethylene glycol monooleate by coordination at poly- glyoxal class list
Oleic acid ester compounds, under the catalysis of N-chlorosuccinimide, poly- glyoxal class monoleate compound chlorination is poly- second two
Acyl chlorides monoleate shows that poly- ethanedioly chloride monoleate forms friendship between polyethylene glycol monooleate polymer by experiment
It is associated, make polyethylene glycol monooleate polymer that there is stable electric conductivity, so that coating be made to have the function of antistatic.
Preferably, the antioxidant compound is four (2,4- di-tert-butylphenol) -4,4'- xenyl diphosphites,
Preventing polyethylene glycol monooleate to be oxidized makes fire retardant fail.
Preferably, the organic silicon flame-retardant adjuvant is the polysiloxane-based fire-retardant adjuvant of carboxyl.
Preferably, the polyethylene glycol monooleate halogen-free flame retardants of the antistatic, preparation method the following steps are included:
(1) 50-60 parts of polyethylene glycol monooleates are weighed, is added in 500mL beaker, adds 200ml ethyl alcohol, then weigh
0.3-0.8 parts of antioxidant compounds and 40-50 parts of organic silicon flame-retardant adjuvants, sequentially add in beaker, heating water bath to 80-
85 DEG C, 0.5-1h is quickly stirred, constantly adds ethyl alcohol in whipping process, maintaining amount of solution makes 200mL, answers antioxidant
It closes object and organic silicon flame-retardant adjuvant is sufficiently uniformly mixed with polyethylene glycol monooleate；
(2) it weighs 0.1-0.3 parts of collaboration metal-non-metal catalyst to be added in above-mentioned steps (1) solution, heating water bath is extremely
40 DEG C, at the uniform velocity stirring 2-3h, make a small amount of polyethylene glycol monooleate generate a small amount of poly- ethanedioly chloride through peroxidating and halogenation
Monoleate；
(3) material in above-mentioned steps (2) is cooled to room temperature, by vacuum distillation, obtains preventing by 300 mesh mesh screens quiet
The polyethylene glycol monooleate halogen-free flame retardants of electricity.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
1, the cellulose base halogen-free flame retardants of the insulating properties passes through polyethylene glycol monooleate and organic silicon flame-retardant adjuvant
Crosslinking becomes compound, without toxic halogen element, and effectively improves the anti-flammability of material, while will not influence material
Thermal conductivity.
2, the cellulose base halogen-free flame retardants of the insulating properties, collaboration metal-non-metal catalyst are bis cyclopentadienyl zirconium dichloride and N-
The compound of bromosuccinimide, by bis cyclopentadienyl zirconium dichloride, by a small amount of polyethylene glycol monooleate by coordination at poly- second two
Aldehydes monoleate compound, under the catalysis of N-chlorosuccinimide, poly- glyoxal class monoleate compound chlorination is
Poly- ethanedioly chloride monoleate shows poly- ethanedioly chloride monoleate between polyethylene glycol monooleate polymer by experiment
Crosslinking band is formed, makes polyethylene glycol monooleate polymer that there is stable electric conductivity, to make coating that there is antistatic
Function.
Specific embodiment
A kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic, the raw material including following parts by weight proportion,
Be characterized in that: 50-60 parts of polyethylene glycol monooleates, 0.3-0.8 parts of antioxidant compounds, 40-50 parts of organic silicon flame-retardants are auxiliary
Auxiliary agent, 0.1-0.3 parts of collaboration metal-non-metal catalyst, polyethylene glycol monooleate are the polymer of oleic acid and polyethylene glycol,
Preparation method is as follows:
(1) 20g oleic acid and 50mL1 are weighed, 4- dioxane is sequentially placed into 500mL beaker, adds 35g polyethylene glycol
With 2g catalyst benzene sulfonic acid, then heating water bath is to 70 DEG C, at the uniform velocity stirring 12h；
(2) it after fully reacting, is cooled to room temperature, 5 sodium bicarbonates is added into the beaker of above-mentioned steps (1), at the uniform velocity stir
20-30min neutralizes benzene sulfonic acid；
(3) 40g polyethylene glycol is added to be extracted, vacuum distillation removes Isosorbide-5-Nitrae-dioxane after extraction, filters crude product
Obtain polyethylene glycol monooleate.
Cooperateing with metal-non-metal catalyst is the compound of bis cyclopentadienyl zirconium dichloride and N-bromosuccinimide, mass ratio
For 6:1.By bis cyclopentadienyl zirconium dichloride, by a small amount of polyethylene glycol monooleate by coordination at poly- glyoxal class monoleate chemical combination
Object, under the catalysis of N-chlorosuccinimide, poly- glyoxal class monoleate compound chlorination is poly- ethanedioly chloride list oleic acid
Ester shows that poly- ethanedioly chloride monoleate forms crosslinking band between polyethylene glycol monooleate polymer by experiment, makes to gather
Ethylene glycol monoleate polymer has stable electric conductivity, so that coating be made to have the function of that antistatic, antioxidant are multiple
Conjunction object is four (2,4- di-tert-butylphenol) -4,4'- xenyl diphosphites, and preventing polyethylene glycol monooleate to be oxidized makes to hinder
Agent failure is fired, the organic silicon flame-retardant adjuvant is the polysiloxane-based fire-retardant adjuvant of carboxyl, the polyethyleneglycol oil of antistatic
Acid esters halogen-free flame retardants, preparation method the following steps are included:
(1) 50-60 parts of polyethylene glycol monooleates are weighed, is added in 500mL beaker, adds 200ml ethyl alcohol, then weigh
0.3-0.8 parts of antioxidant compounds and 40-50 parts of organic silicon flame-retardant adjuvants, sequentially add in beaker, heating water bath to 80-
85 DEG C, 0.5-1h is quickly stirred, constantly adds ethyl alcohol in whipping process, maintaining amount of solution makes 200mL, answers antioxidant
It closes object and organic silicon flame-retardant adjuvant is sufficiently uniformly mixed with polyethylene glycol monooleate；
(2) it weighs 0.1-0.3 parts of collaboration metal-non-metal catalyst to be added in above-mentioned steps (1) solution, heating water bath is extremely
40 DEG C, at the uniform velocity stirring 2-3h, make a small amount of polyethylene glycol monooleate generate a small amount of poly- ethanedioly chloride through peroxidating and halogenation
Monoleate；
(3) material in above-mentioned steps (2) is cooled to room temperature, by vacuum distillation, obtains preventing by 300 mesh mesh screens quiet
The polyethylene glycol monooleate halogen-free flame retardants of electricity.
Embodiment 1:
(1) 50 parts of polyethylene glycol monooleates are weighed, is added in 500mL beaker, adds 200ml ethyl alcohol, then weigh 0.3
Part antioxidant compound and 40 parts of organic silicon flame-retardant adjuvants, sequentially add in beaker, heating water bath is to 80-85 DEG C, quickly
0.5-1h is stirred, constantly adds ethyl alcohol in whipping process, maintaining amount of solution makes 200mL, makes antioxidant compound and has
The fire-retardant adjuvant of machine silicon is sufficiently uniformly mixed with polyethylene glycol monooleate；
(2) it weighs 0.1 part of collaboration metal-non-metal catalyst to be added in above-mentioned steps (1) solution, heating water bath to 40
DEG C, at the uniform velocity stirring 2-3h makes a small amount of polyethylene glycol monooleate generate a small amount of poly- ethanedioly chloride list through peroxidating and halogenation
Oleate；
(3) material in above-mentioned steps (2) is cooled to room temperature, by vacuum distillation, obtains preventing by 300 mesh mesh screens quiet
The polyethylene glycol monooleate halogen-free flame retardants component 1 of electricity.
Embodiment 2:
(1) 55 parts of polyethylene glycol monooleates are weighed, is added in 500mL beaker, adds 200ml ethyl alcohol, then weigh 0.3
Part antioxidant compound and 45 parts of organic silicon flame-retardant adjuvants, sequentially add in beaker, heating water bath is to 80-85 DEG C, quickly
0.5-1h is stirred, constantly adds ethyl alcohol in whipping process, maintaining amount of solution makes 200mL, makes antioxidant compound and has
The fire-retardant adjuvant of machine silicon is sufficiently uniformly mixed with polyethylene glycol monooleate；
(2) it weighs 0.1 part of collaboration metal-non-metal catalyst to be added in above-mentioned steps (1) solution, heating water bath to 40
DEG C, at the uniform velocity stirring 2-3h makes a small amount of polyethylene glycol monooleate generate a small amount of poly- ethanedioly chloride list through peroxidating and halogenation
Oleate；
(3) material in above-mentioned steps (2) is cooled to room temperature, by vacuum distillation, obtains preventing by 300 mesh mesh screens quiet
The polyethylene glycol monooleate halogen-free flame retardants component 2 of electricity.
Embodiment 3:
(1) 55 parts of polyethylene glycol monooleates are weighed, is added in 500mL beaker, adds 200ml ethyl alcohol, then weigh 0.6
Part antioxidant compound and 45 parts of organic silicon flame-retardant adjuvants, sequentially add in beaker, heating water bath is to 80-85 DEG C, quickly
0.5-1h is stirred, constantly adds ethyl alcohol in whipping process, maintaining amount of solution makes 200mL, makes antioxidant compound and has
The fire-retardant adjuvant of machine silicon is sufficiently uniformly mixed with polyethylene glycol monooleate；
(2) it weighs 0.3 part of collaboration metal-non-metal catalyst to be added in above-mentioned steps (1) solution, heating water bath to 40
DEG C, at the uniform velocity stirring 2-3h makes a small amount of polyethylene glycol monooleate generate a small amount of poly- ethanedioly chloride list through peroxidating and halogenation
Oleate；
(3) material in above-mentioned steps (2) is cooled to room temperature, by vacuum distillation, obtains preventing by 300 mesh mesh screens quiet
The polyethylene glycol monooleate halogen-free flame retardants component 3 of electricity.
Claims (6)
1. a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic, the raw material including following parts by weight proportion is special
Sign is: 50-60 parts of polyethylene glycol monooleates, 0.3-0.8 parts of antioxidant compounds, 40-50 parts of organic silicon flame-retardant auxiliary
Agent, 0.1-0.3 parts of collaboration metal-non-metal catalyst.
2. a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic according to claim 1, it is characterised in that: institute
The polymer that polyethylene glycol monooleate is oleic acid and polyethylene glycol is stated, preparation method is as follows:
(1) 20g oleic acid and 50mL1 are weighed, 4- dioxane is sequentially placed into 500mL beaker, adds 35g polyethylene glycol and 2g
Catalyst benzene sulfonic acid, then heating water bath is to 70 DEG C, at the uniform velocity stirring 12h；
(2) it after fully reacting, is cooled to room temperature, 5 sodium bicarbonates is added into the beaker of above-mentioned steps (1), at the uniform velocity stirring 20-
30min neutralizes benzene sulfonic acid；
(3) 40g polyethylene glycol is added to be extracted, vacuum distillation removes Isosorbide-5-Nitrae-dioxane after extraction, and filtering crude product obtains
Polyethylene glycol monooleate.
3. a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic according to claim 1, it is characterised in that: institute
State the compound that collaboration metal-non-metal catalyst is bis cyclopentadienyl zirconium dichloride and N-bromosuccinimide, mass ratio 6:1.
By bis cyclopentadienyl zirconium dichloride, by a small amount of polyethylene glycol monooleate by coordination at poly- glyoxal class monoleate compound, in N-
Under the catalysis of chlorosuccinimide, poly- glyoxal class monoleate compound chlorination is poly- ethanedioly chloride monoleate, is passed through
Experiment shows that poly- ethanedioly chloride monoleate forms crosslinking band between polyethylene glycol monooleate polymer, makes polyethyleneglycol
Oleic acid ester polymer has stable electric conductivity, so that coating be made to have the function of antistatic.
4. a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic according to claim 1, it is characterised in that: institute
Stating antioxidant compound is four (2,4- di-tert-butylphenol) -4,4'- xenyl diphosphites, prevents polyethyleneglycol oleic acid
Ester, which is oxidized, makes fire retardant fail.
5. a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic according to claim 1, it is characterised in that: institute
Stating organic silicon flame-retardant adjuvant is the polysiloxane-based fire-retardant adjuvant of carboxyl.
6. a kind of polyethylene glycol monooleate halogen-free flame retardants of antistatic according to claim 1, which is characterized in that institute
State the polyethylene glycol monooleate halogen-free flame retardants of antistatic, preparation method the following steps are included:
(1) 50-60 parts of polyethylene glycol monooleates are weighed, is added in 500mL beaker, adds 200ml ethyl alcohol, then weigh 0.3-
0.8 part of antioxidant compound and 40-50 parts of organic silicon flame-retardant adjuvants, sequentially add in beaker, heating water bath to 80-85
DEG C, 0.5-1h is quickly stirred, constantly adds ethyl alcohol in whipping process, maintaining amount of solution makes 200mL, keeps antioxidant compound
Object and organic silicon flame-retardant adjuvant are sufficiently uniformly mixed with polyethylene glycol monooleate；
(2) it weighs 0.1-0.3 parts of collaboration metal-non-metal catalyst to be added in above-mentioned steps (1) solution, heating water bath to 40
DEG C, at the uniform velocity stirring 2-3h makes a small amount of polyethylene glycol monooleate generate a small amount of poly- ethanedioly chloride list through peroxidating and halogenation
Oleate；
(3) material in above-mentioned steps (2) is cooled to room temperature, by vacuum distillation, obtains antistatic by 300 mesh mesh screens
Polyethylene glycol monooleate halogen-free flame retardants.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591435A (en) * | 2019-10-16 | 2019-12-20 | 厦门芒娅贸易有限公司 | Antistatic polyethylene glycol monooleate halogen-free flame retardant |
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2019
- 2019-07-10 CN CN201910621608.9A patent/CN110305512A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591435A (en) * | 2019-10-16 | 2019-12-20 | 厦门芒娅贸易有限公司 | Antistatic polyethylene glycol monooleate halogen-free flame retardant |
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Application publication date: 20191008 |