CN110183728A - A kind of in-situ polymerization expansion type flame retardant and prepare raw material and its preparation method and application - Google Patents
A kind of in-situ polymerization expansion type flame retardant and prepare raw material and its preparation method and application Download PDFInfo
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- CN110183728A CN110183728A CN201910574046.7A CN201910574046A CN110183728A CN 110183728 A CN110183728 A CN 110183728A CN 201910574046 A CN201910574046 A CN 201910574046A CN 110183728 A CN110183728 A CN 110183728A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to flame retardant area, discloses a kind of in-situ polymerization expansion type flame retardant and prepare raw material and its preparation method and application.The preparation method of the in-situ polymerization expansion type flame retardant includes: S1, concentrated acid and crystalline flake graphite is stirred 30~60min at 30~40 DEG C, and gained mixture is ultrasonically treated 20~100min later, obtains swelling crystalline flake graphite；S2, crystalline flake graphite will be swollen and contain compound nitrogen series and carry out in-situ polymerization containing phosphorus series compound, and gained in-situ polymerization product will be separated by solid-liquid separation later, and obtained solid product is washed and dried, obtain intercalated graphite；S3, intercalated graphite and boride are uniformly mixed.Has the characteristics that Halogen, environmental protection, nontoxic, efficient, without dripping off using in-situ polymerization expansion type flame retardant obtained by method provided by the invention, it can not only be effectively fire-retardant for polyolefin, and it is good with polyolefin-based compatability, influence is basically will not produce on its mechanical performance.
Description
Technical field
The invention belongs to flame retardant areas, and in particular to a kind of in-situ polymerization expansion type flame retardant and prepare raw material and its system
Preparation Method and application.
Background technique
Fire retardant is widely used in vapour as the world's second largest high molecular material additive for being only second to plasticizer at present
The all trades and professions such as vehicle, household electrical appliances, electrotechnical, electronic, space flight and aviation, health care, building.Every annual consumption of fire retardant is up to 200,000 tons
More than, wherein 80% is halogenated flame retardant.However, halogenated flame retardant in burning there is murder by poisoning, dense smoke, drippage, environmental protection etc. to ask
Topic, since 2006, European Union limited the use of a plurality of halogenated flame retardants, such as octa-BDE, penta-BDE, and other
Though halogenated flame retardant is not limited, as environmental issue is increasingly serious and prominent, halogenated flame retardant exits history dance at last
Platform instead will be non-toxic, the efficient and good and moderate halogen-free flame retardants of matrix compatibility.
Currently, common halogen-free flame retardants has phosphorus flame retardant, nitrogenated flame retardant, phosphorus-nitrogenated flame retardant etc., but it is existing
Halogen-free flame retardants exist with matrix poor compatibility, be easily precipitated, additive amount is big, the problems such as easily deliquescing, flame retardant property and and base
Compatability still needs to be further increased.
Summary of the invention
The purpose of the invention is to overcome existing halogen-free flame retardants flame retardant effect poor and with matrix compatibility compared with
The defect of difference, and provide it is a kind of have good flame retardant effect and with matrix compatibility it is good, will not influence matrix mechanical performance substantially
In-situ polymerization expansion type flame retardant and prepare raw material and its preparation method and application.
Specifically, raw material is prepared the present invention provides a kind of in-situ polymerization expansion type flame retardant, wherein the original position is poly-
The raw material for preparing for closing expansion type flame retardant consists of the following components in percentage by weight:
Preferably, the concentrated acid is selected from least one of concentrated phosphoric acid, the concentrated sulfuric acid, concentrated nitric acid and dense chromic acid.
Preferably, the concentration of the concentrated acid is 98wt% or more.
Preferably, the carbon content of the crystalline flake graphite is 87wt% or more.
Preferably, the partial size of the crystalline flake graphite is 80~100 mesh.
Preferably, the compound nitrogen series that contain are ammonium class compound and/or amides compound, are more preferably selected from phosphinylidyne
At least one of amine, polyurethane, double focusing cyanamide, melamine and carbamide resin.
Preferably, described to be selected from ammonium phosphate salt, phosphate, ammonium polyphosphate, polyphosphoric acid amide, Ji Wusi containing phosphorus series compound
At least one of alcohol phosphate ester melamine salt, Melamine Polyphosphate and melamine phosphate.
Preferably, the boride is selected from least one of zinc borate, line borate and aluminium borate.
The present invention also provides a kind of preparation methods of in-situ polymerization expansion type flame retardant, wherein this method is with above-mentioned original
Position polymerization expansion type flame retardant prepare raw material as raw material and the following steps are included:
S1, the concentrated acid and crystalline flake graphite are stirred 30~60min at 30~40 DEG C, later by gained mixture
It is ultrasonically treated 20~100min, obtains swelling crystalline flake graphite；
S2, by the swelling crystalline flake graphite and it is described containing compound nitrogen series and containing phosphorus series compound carry out in-situ polymerization, it
Gained in-situ polymerization product is separated by solid-liquid separation afterwards, and obtained solid product is washed and dried, obtains intercalated graphite；
S3, the intercalated graphite and the boride are uniformly mixed.
Preferably, in step S2, the condition of the in-situ polymerization includes that temperature is 40~50 DEG C, and the time is 30~60min.
Preferably, in step S2, the condition of the washing makes the pH value 7~8 of washed product.
Preferably, in step S2, the condition of the drying includes that temperature is 50~65 DEG C, and the time is 30~50min.
The present invention also provides in-situ polymerization expansion type flame retardants prepared by the above method.
In addition, the application the present invention also provides the in-situ polymerization expansion type flame retardant as polyolefine fire retardant.
The present invention is ultrasonically treated after being first stirred concentrated acid and crystalline flake graphite, using concentrated acid that crystalline flake graphite lamella is molten
Swollen opening adds intercalation object containing compound nitrogen series and containing phosphorus series compound later and carries out in-situ polymerization, finally mixes again with boride
It is fire-retardant that compounding carries out synergistic, and thus obtained in-situ polymerization expansion type flame retardant has Halogen, environmental protection, nontoxic, efficient, without dripping off
The features such as, it can not only be effectively fire-retardant and good with polyolefin-based compatability for polyolefin, substantially not to its mechanical performance
It can have an impact.
Fire-retardant principle of the invention is in 300 DEG C or so when the in-situ polymerization expansion type flame retardant to fire-retardant environment
When middle, be adsorbed on crystalline flake graphite piece interlayer containing compound nitrogen series and gas, scale stone can be thermally decomposed into containing phosphorus series compound
The black hundred times that can swell moment, the nitrogen energy that oxygen can be effectively isolated and enter and imflammable gas is inhibited to escape, while being generated
It reaches oxygen concentration in diluent air and reduces material surface temperature, then be equipped with boride to generate borate salt, promote wait hinder
At carbon, it includes that solidifying phase is fire-retardant gentle mutually fire-retardant fire-retardant which is a kind of simultaneously on combustion things surface
Agent.
Specific embodiment
There is no particular limitation for type of the present invention to concentrated acid, can for it is existing it is various can be molten by crystalline flake graphite lamella
The high concentration acid solution of swollen opening, specific example includes but is not limited to: in concentrated phosphoric acid, the concentrated sulfuric acid, concentrated nitric acid and dense chromic acid extremely
Few one kind.The concentration of the concentrated acid is preferably 98wt% or more.
The graphite crystal of the crystalline flake graphite is in flakey.The carbon content of the crystalline flake graphite is preferably 87wt% or more,
More preferably 90~95wt%.That is, the crystalline flake graphite is preferably medium-carbon graphite, high-carbon graphite or high purity graphite.The scale
The partial size of graphite is preferably 80~100 mesh.
There is no particular limitation to the type containing compound nitrogen series by the present invention, can for it is existing it is various being capable of conduct
Intercalation object enters in crystalline flake graphite lamella and the heated substance for being decomposed into nitrogen, such as can be ammonium class compound and/or amide
Class compound, specific example include but is not limited to: in carbamide, polyurethane, double focusing cyanamide, melamine and carbamide resin
It is at least one.
In the present invention, the role containing phosphorus series compound is to promote to flame retardant surface dewatering at carbon, in height
Temperature effect is lower react at carbon with carbon source (resin), promotes molten system foaming and intumescing, oxygen and fuel gas reaction is isolated,
Burning is further suppressed, specific example includes but is not limited to: ammonium phosphate salt, phosphate, ammonium polyphosphate, polyphosphoric acid amide, season
At least one of penta tetrol phosphate ester melamine salt, Melamine Polyphosphate and melamine phosphate.
It needs, when used raw material is not only nitrogenous but also phosphorous compound, the content of the raw material should be included in
Content containing phosphorus series compound.
There is no particular limitation for type of the present invention to the boride, can be selected from zinc borate, line borate and aluminium borate
At least one of.
The preparation method of in-situ polymerization expansion type flame retardant provided by the invention is with above-mentioned in-situ polymerization expansion type flame retardant
Prepare raw material as raw material and the following steps are included:
S1, the concentrated acid and crystalline flake graphite are stirred 30~60min at 30~40 DEG C, later by gained mixture
It is ultrasonically treated 20~100min, obtains swelling crystalline flake graphite；
S2, by the swelling crystalline flake graphite and it is described containing compound nitrogen series and containing phosphorus series compound carry out in-situ polymerization, it
Gained in-situ polymerization product is separated by solid-liquid separation afterwards, and obtained solid product is washed and dried, obtains intercalated graphite；
S3, the intercalated graphite and the boride are uniformly mixed.
Specific reaction process is as follows: crystalline flake graphite first open under concentrated acid effect by lamella swelling, and nitrogenous systemization is added later
It closes object and contains phosphorus series compound, both substances can enter in the lamellar structure of crystalline flake graphite as intercalation object, form oxidation stone
Ink is capable of forming extensive chemical by the group effect between them and combines, and when by high temperature action, these compounds can be fast
Speed resolves into gas, and further swell graphite, thus reach fire retardation, and last mixed boride can play synergistic resistance
Combustion effect.
In the present invention, in step S1, supersonic frequency used by the ultrasonic treatment can be 20~50KHz.
In the present invention, in step S2, it is 40~50 DEG C that the condition of the in-situ polymerization, which preferably includes temperature, the time 30
~60min.The mode of the separation of solid and liquid can be for example suction filtration, filters pressing etc..Detergent used by the washing is preferably
Lye is specifically as follows in sodium hydroxide solution, potassium hydroxide solution, sodium bicarbonate solution, potassium bicarbonate solution etc. at least
It is a kind of.The time of the washing, which is preferably subject to, ensures the pH value of washed product to 7~8.The condition of the drying generally includes
Temperature can be 50~65 DEG C, and the time can be 30~50min.
In the present invention, in step S3, the mixed condition generally includes temperature can be for room temperature, and stirring rate can be with
For 80~130rpm, the time can be 20~40min.
The present invention also provides in-situ polymerization expansion type flame retardants prepared by the above method.
In addition, the application the present invention also provides the in-situ polymerization expansion type flame retardant as polyolefine fire retardant.Its
In, the polyolefin for example can be in polypropylene, polyethylene, poly 1-butene, poly- 2- butylene, polybutadiene, polystyrene etc.
At least one.
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot
It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, described according to the literature in the art
Technology or conditions or carried out according to product description.Reagents or instruments used without specified manufacturer is that can lead to
Cross the conventional products of commercially available acquisition.
Embodiment 1
The embodiment is used to illustrate the preparation of in-situ polymerization expansion type flame retardant provided by the invention, wherein each raw material
Dosage is as shown in table 1, and detailed process is as follows:
S1, by concentrated acid (concentrated phosphoric acid that concentration is 98wt%) and crystalline flake graphite (carbon content be 90wt% and partial size be 80~
100 mesh) it is added in the three-neck flask equipped with condenser pipe, 60min is stirred at 30 DEG C, later by gained mixture in frequency
100min is handled in the ultrasonic wave that rate is 30KHz, obtains swelling crystalline flake graphite；
S2, swelling crystalline flake graphite is poured into equipped with containing compound nitrogen series (carbamide) and (melamine containing phosphorus series compound
Phosphate) flask in and at 40 DEG C stir 60min to complete in-situ polymerization, gained in-situ polymerization product is taken out later
Filter, filter residue alkali liquid washing to pH value are 7, then gained washed product is placed at 65 DEG C of temperature dry 30min, obtain intercalation stone
Ink；
S3, intercalated graphite is added in boride (zinc borate), high-speed stirred 30min obtains in-situ polymerization intumescent
Fire retardant.
Embodiment 2
The embodiment is used to illustrate the preparation of in-situ polymerization expansion type flame retardant provided by the invention, wherein each raw material
Dosage is as shown in table 1, and detailed process is as follows:
S1, by concentrated acid (concentrated sulfuric acid that concentration is 98wt%) and crystalline flake graphite (carbon content be 95wt% and partial size be 80~
It is more than 100 mesh) it is added in the three-neck flask equipped with condenser pipe, 30min is stirred at 40 DEG C, later by gained mixture
60min is handled in the ultrasonic wave that frequency is 30Hz, obtains swelling crystalline flake graphite；
S2, swelling crystalline flake graphite is poured into equipped with containing compound nitrogen series (carbamide resin) and (orthophosphoric acid containing phosphorus series compound
Ester) flask in and at 50 DEG C stir 30min to complete in-situ polymerization, gained in-situ polymerization product is filtered later,
Filter residue alkali liquid washing to pH value is 8, then gained washed product is placed under temperature 50 C dry 50min, obtains intercalated graphite；
S3, intercalated graphite is added in boride (line borate), high-speed stirred 30min obtains in-situ polymerization intumescent
Fire retardant.
Embodiment 3
The embodiment is used to illustrate the preparation of in-situ polymerization expansion type flame retardant provided by the invention, wherein each raw material
Dosage is as shown in table 1, and detailed process is as follows:
S1, by concentrated acid (concentrated nitric acid that concentration is 98wt%) and crystalline flake graphite (carbon content be 92wt% and partial size be 80~
It is more than 100 mesh) it is added in the three-neck flask equipped with condenser pipe, 45min is stirred at 35 DEG C, later by gained mixture
20min is handled in the ultrasonic wave that frequency is 50Hz, obtains swelling crystalline flake graphite；
S2, swelling crystalline flake graphite is poured into equipped with containing compound nitrogen series (polyurethane) and (tripolyphosphate containing phosphorus series compound
Ammonium) flask in and at 45 DEG C stir 45min to complete in-situ polymerization, gained in-situ polymerization product is filtered later,
Filter residue alkali liquid washing to pH value is 7.5, and gained washed product is placed at 55 DEG C of temperature dry 40min later, obtains intercalation
Graphite；
S3, intercalated graphite is added in boride (aluminium borate), high-speed stirred 30min obtains in-situ polymerization intumescent
Fire retardant.
Embodiment 4
The embodiment is used to illustrate the preparation of in-situ polymerization expansion type flame retardant provided by the invention, wherein each raw material
Dosage is as shown in table 1, and detailed process is as follows:
S1, by concentrated acid (the dense chromic acid that concentration is 98wt%) and crystalline flake graphite (carbon content be 90wt% and partial size be 80~
100 mesh) it is added in the three-neck flask equipped with condenser pipe, 45min is stirred at 35 DEG C, later by gained mixture in frequency
60min is handled in the ultrasonic wave that rate is 50Hz, obtains swelling crystalline flake graphite；
S2, swelling crystalline flake graphite is poured into equipped with containing compound nitrogen series (double focusing cyanamide) and (Ji Wusi containing phosphorus series compound
Alcohol phosphate ester melamine salt) flask in and at 45 DEG C stir 45min to complete in-situ polymerization, gained in-situ polymerization is produced later
Object is filtered, and filter residue alkali liquid washing to pH value is 7.5, gained washed product is placed at 65 DEG C of temperature later dry
30min obtains intercalated graphite；
S3, intercalated graphite is added in boride (zinc borate), high-speed stirred 30min obtains in-situ polymerization intumescent
Fire retardant.
Comparative example 1
In-situ polymerization expansion type flame retardant is prepared according to the method for embodiment 1, unlike, boride and part are contained
Phosphorus series compound is substituted using the concentrated acid of identical weight part, remaining condition is same as Example 1, obtains the expansion of reference in-situ polymerization
Type fire retardant.Wherein, the dosage of each substance is as shown in table 1.
Comparative example 2
In-situ polymerization expansion type flame retardant is prepared according to the method for embodiment 1, unlike, the dosage of each substance is not at this
In the range of invention, remaining condition is same as Example 1, obtains reference in-situ polymerization expansion type flame retardant.Wherein, each substance
Dosage is as shown in table 1.
Comparative example 3
In-situ polymerization expansion type flame retardant is prepared according to the method for embodiment 1, unlike, by boride using identical heavy
The crystalline flake graphite substitution of part is measured, remaining condition is same as Example 1, obtains reference in-situ polymerization expansion type flame retardant.Wherein, respectively
The dosage of substance is as shown in table 1.
Comparative example 4
In-situ polymerization expansion type flame retardant is prepared according to the method for embodiment 1, unlike, compound nitrogen series use will be contained
Identical weight part substitutes containing phosphorus series compound, remaining condition is same as Example 1, obtains reference in-situ polymerization expansion type flame-retarding
Agent.Wherein, the dosage of each substance is as shown in table 1.
1 raw material dosage of table (wt%)
Test case
By the in-situ polymerization expansion type flame retardant obtained by Examples 1 to 4 and the reference original obtained by comparative example 1~4
Position polymerization expansion type flame retardant is added to polypropylene (trade mark 7726H, pure LOI according to the ratio of 24wt% and 30wt% respectively
18%, UL94V-2 are 11.8kJ/m according to the Izod notched impact strength that GB/T 1843-2008 standard measures2) in, institute
Izod notched impact strength, LOI oxygen index (OI) and the flame retardant property for obtaining composite material are tested in accordance with the following methods, gained
The results are shown in Table 2.
(1) it Izod notched impact strength: is tested according to GB/T 1843-2008 standard；
(2) it LOI oxygen index (OI): is tested according to GB/T 2406.2-2009 standard；
(3) it flame retardant property: is tested according to UL94 standard, wherein sample thickness 3.2mm.
Table 2
From the results shown in Table 2, fire retardant additive amount is the corresponding oxygen of 24wt% and 30wt% in Examples 1 to 4
Index (LOI) has respectively reached 28.2%~30.7% and 29.6%~32.1%, hence it is evident that higher than comparative example 1~4
24.4%~26.2% and 25.5%~27.1%；And the flame retardant rating of embodiment has entirely reached V-0 grades, is higher than comparative example
V-1 grade in 1~4 and V-2 grades；Simultaneously using in-situ polymerization expansion type flame retardant provided by the invention to composite polyolefine material
Izod notched impact strength do not influence substantially.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (10)
1. a kind of in-situ polymerization expansion type flame retardant prepares raw material, which is characterized in that the in-situ polymerization expansion type flame retardant
The raw material for preparing consist of the following components in percentage by weight:
2. in-situ polymerization expansion type flame retardant according to claim 1 prepares raw material, which is characterized in that the concentrated acid choosing
From at least one of concentrated phosphoric acid, the concentrated sulfuric acid, concentrated nitric acid and dense chromic acid；The concentration of the concentrated acid is 98wt% or more.
3. in-situ polymerization expansion type flame retardant according to claim 1 prepares raw material, which is characterized in that the scale stone
The carbon content of ink is 87wt% or more；The partial size of the crystalline flake graphite is 80~100 mesh.
4. in-situ polymerization expansion type flame retardant according to claim 1 prepares raw material, which is characterized in that the nitrogenous system
Compound be ammonium class compound and/or amides compound, be preferably selected from carbamide, polyurethane, double focusing cyanamide, melamine and
At least one of carbamide resin.
5. in-situ polymerization expansion type flame retardant according to claim 1 prepares raw material, which is characterized in that the phosphorous system
It is more that compound is selected from ammonium phosphate salt, phosphate, ammonium polyphosphate, polyphosphoric acid amide, pentaerythritol phosphate melamine salt, melamine
At least one of Quadrafos and melamine phosphate.
6. in-situ polymerization expansion type flame retardant according to claim 1 prepares raw material, which is characterized in that the boride
Selected from least one of zinc borate, line borate and aluminium borate.
7. a kind of preparation method of in-situ polymerization expansion type flame retardant, which is characterized in that this method in claim 1~6 to appoint
Meaning one described in in-situ polymerization expansion type flame retardant prepare raw material as raw material and the following steps are included:
S1, the concentrated acid and crystalline flake graphite are stirred 30~60min at 30~40 DEG C, later by gained mixture ultrasound
20~100min is handled, swelling crystalline flake graphite is obtained；
S2, by the swelling crystalline flake graphite and it is described containing compound nitrogen series and containing phosphorus series compound carry out in-situ polymerization, later will
Gained in-situ polymerization product is separated by solid-liquid separation, and obtained solid product is washed and dried, and obtains intercalated graphite；
S3, the intercalated graphite and the boride are uniformly mixed, obtain the in-situ polymerization expansion type flame retardant.
8. the preparation method of in-situ polymerization expansion type flame retardant according to claim 7, which is characterized in that in step S2,
The condition of the in-situ polymerization includes that temperature is 40~50 DEG C, and the time is 30~60min；The condition of the washing makes washed product
PH value be 7~8；The condition of the drying includes that temperature is 50~65 DEG C, and the time is 30~50min.
9. the in-situ polymerization expansion type flame retardant that the method as described in claim 7 or 8 is prepared.
10. application of the in-situ polymerization expansion type flame retardant as claimed in claim 9 as polyolefine fire retardant.
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| CN116589779A (en) * | 2023-07-19 | 2023-08-15 | 山东艾科高分子材料有限公司 | Polyolefin halogen-free flame-retardant master batch |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116589779A (en) * | 2023-07-19 | 2023-08-15 | 山东艾科高分子材料有限公司 | Polyolefin halogen-free flame-retardant master batch |
| CN116589779B (en) * | 2023-07-19 | 2023-09-12 | 山东艾科高分子材料有限公司 | Polyolefin halogen-free flame-retardant master batch |
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