CN109912842A - A kind of preparation and application of efficient microcapsules composite flame-retardant agent - Google Patents
A kind of preparation and application of efficient microcapsules composite flame-retardant agent Download PDFInfo
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Abstract
The invention discloses a kind of preparation and application of efficient microcapsules composite flame-retardant agent, are related to technical field of flame retardant.The present invention first absorbs into II type ammonium polyphosphate on the basic magnesium carbonate of flower ball-shaped in micron-sized gap, then the basic magnesium carbonate of II type ammonium polyphosphate has been adsorbed with melamine formaldehyde resin cladding, prepares a kind of efficient microcapsules composite flame-retardant agent.The present invention is first adsorbed ammonium polyphosphate using the basic magnesium carbonate of flower ball-shaped, and the compounding ingredients of acquired special construction recycle melamine formaldehyde resin to be coated as core material, and flame retarding efficiency is higher, gives full play to the synergistic effect of different component.
Description
Technical field:
The present invention relates to technical field of flame retardant, and in particular to a kind of preparation of efficient microcapsules composite flame-retardant agent with answer
With.
Background technique:
Fire retardant can assign combustible polymers fire retardant property.In conventional flame retardant type, inorganic fire retardants is fire-retardant
Inefficient, additive amount is larger, poor with the compatibility of high molecular material, influences the processing and mechanical property of high molecular material.
There are many halogenated flame retardant itself (especially bromine system) chronic toxicity, and it is heated when to generate a large amount of toxic gas harmful to human strong
Health, pollution environment.Expansible graphite is the fire retardant of function admirable in element fire retardant, only traditional expansible graphite due to
The shortcomings that production technology and have very high sulfur content, toxic sulfur oxide gas can be released in high-temperature expansion.And
There are many drawbacks in red phosphorus, such as the easy moisture absorption, oxidizable, dust generation explosive etc. in practical applications.
Phosphorus-nitrogen containing flame retardant is a kind of novel expansion type flame retardant, has good thermal stability and higher anti-flammability
Energy.Wherein being most widely used with II type ammonium polyphosphate (APP).But its there are water resistances poor, single fire retardant pair
In such as PP, PE etc. more inflammable olefin polymer it is fire-retardant poor the disadvantages of.
To overcome the above disadvantages, many research and utilization microcapsule coateds and with other auxiliary agents be used cooperatively modified polyphosphoric acid
Ammonium, such as: number of patent application is that the patent of invention of CN201610765674.X discloses a kind of epoxy resin coated ammonium polyphosphate
The preparation method of microcapsule flame retardant, it is good to have obtained stability, the lower microcapsule flame retardant of water-soluble.Number of patent application is
The patent of invention of CN201310730885.6 discloses a kind of composite flame-retardant agent and system containing microcapsule coated expanding fire retardant
Preparation Method, expanding fire retardant, fire retarding synergist and smoke suppressant is compound, recycle Lauxite or melamine formaldehyde resin
It is coated, obtained fire retardant preferably improves the flame retardant effect of material.These invention disclosed patents only will
Different component is simply compound in flame-retardant system or is coated using resin, and the synergistic for not giving full play to different component is made
With.
Summary of the invention:
Technical problem to be solved by the present invention lies in provide a kind of preparation and application of efficient microcapsules composite flame-retardant agent.
Purpose is by first absorbing into II type ammonium polyphosphate on the basic magnesium carbonate of flower ball-shaped in micron-sized gap, then with three
Paracyanogen amine-formaldehyde resin coats the basic magnesium carbonate for having adsorbed II type ammonium polyphosphate, prepares a kind of efficient microcapsules composite flame-proof
Agent.
Wherein, when adsorbing II type ammonium polyphosphate with the basic magnesium carbonate of flower ball-shaped, since basic carbonate magnesium surface is that band is negative
Electricity, and II type ammonium polyphosphate be also have it is electronegative, so basic magnesium carbonate directly would become hard to the absorption of ammonium polyphosphate
It carries out.To this, we adsorb positively charged cationic surfactant using basic magnesium carbonate first, basic magnesium carbonate table when making
Face has positive charge, then adsorbs ammonium polyphosphate with this.
In addition, the absorption of material is a kind of exothermic process.Basic magnesium carbonate Liquidity limit surfactant and polyphosphoric acid
When ammonium, it should be carried out under the conditions of lower temperature, higher concentration, to increase adsorbance.But since there are molecules for II type ammonium polyphosphate
Interior and intermolecular hydrogen bond, solubility at a lower temperature in water are very low.Ammonium polyphosphate is dissolved in the water at high temperature,
Hydrogen bond existing for destroying inside ammonium polyphosphate, then it is down to room temperature, or be dissolved in the water containing a small amount of NaCl, it can be improved
Solubility at low temperature.
The following technical solution is employed for the technical problems to be solved by the invention to realize:
A kind of preparation of efficient microcapsules composite flame-retardant agent, comprising the following steps:
(1) the II type ammonium polyphosphate of certain mass number is dissolved in the water at high temperature and is down to room temperature or at room temperature again
Be dissolved in the NaCl aqueous solution that mass fraction is 0.5%~2%, be filtered to remove a small amount of insoluble matter obtain high concentration II type it is poly-
Ammonium phosphate solution；
(2) cationic surfactant of certain mass number is dissolved in the water at room temperature, is added under stiring certain
The flower ball-shaped basic magnesium carbonate of mass fraction, and continue stirring 1~5 hour, gained suspension is filtered, filter cake is washed with water to filter
Liquid is neutrality, then filter cake is dried in 80~120 DEG C, obtains the modified flower ball-shaped basic carbonate in cationic surfactant surface
Magnesium；
(3) basic magnesium carbonate obtained by step (2) is added slowly with stirring II type ammonium polyphosphate solution obtained by step (1)
In, and be continuously stirred at room temperature 1~5 hour, gained suspension is filtered, then filter cake is dried in 80~120 DEG C, is inhaled
The attached basic magnesium carbonate of II type ammonium polyphosphate；
(4) melamine of certain mass number and 37% formalin are dissolved in a certain amount of water, are increased the temperature to
It is reacted at 60~95 DEG C 0.5-3 hours, during which keeping system pH with the solution of bronsted lowry acids and bases bronsted lowry is 8~10, is down to after reaction
Room temperature obtains the prepolymer solution of the melamine formaldehyde resin of clear；
(5) by the dispersion of basic magnesium carbonate obtained by step (3) and suspension obtained in solvent, under stiring by step (4) institute
It obtains melamine formaldehyde resin performed polymer to be slowly added in obtained suspension, regulation system pH value is 3~6, is slowly heated up
It is reacted 2~8 hours to 60~90 DEG C, system is cooled to room temperature filtering after reaction, filter cake is washed with water to during filtrate is
Property, then filter cake is dried in 80~120 DEG C, it obtains melamine formaldehyde resin cladding basic magnesium carbonate and ammonium polyphosphate is answered
Close combustion adjuvant, i.e., a kind of efficient microcapsules composite flame-retardant agent；
(6) by microcapsule flame retardant obtained by step (5) and polymeric matrix and lubricant, plasticizer, antioxidant, filler
And other auxiliary agents are sufficiently mixed uniformly with open mill by a certain percentage, prepare batten using Screw Extrusion injection molding machine；
(7) by batten limit of utilization oxygen index measurer, radial-boom impact tester, universal testing machine obtained by step (6)
Measure its oxygen index (OI), notch impact strength, tensile strength etc..
Preferably, step (1), (2), in (4) raw material mass fraction are as follows: 10~20 parts of II type ammonium polyphosphate, step (1)
Middle water or 80~180 parts of aqueous solution containing a small amount of NaCl, 5~20 parts of cationic surfactant, water 60~120 in step (2)
Part, 30~80 parts of basic magnesium carbonate, 5~20 parts of melamine, 37% 5~30 parts of formaldehyde.
Preferably, in step (6) raw material mass fraction are as follows: 15~40 parts of microcapsules composite flame-retardant agent, polymeric matrix
30~50 parts of material, 0.1~3 part of lubricant, 10~30 parts of toughener, 5~30 parts of filler.
Wherein, step (2) described cationic surfactant is selected from but is not limited to: cetyl trimethylammonium bromide,
The quaternary cationic surfactants such as dodecyl benzyl dimethyl ammonium chloride；Cetyl pyridinium bromide, dodecyl
The heterocyclics cationic surfactant such as benzotriazole cationic surfactant；Suo Luoming A, polyethyleneimine amine hydrochlorate etc.
One or more of amine salt cationic surfactant.
The present invention also provides application of the above-mentioned efficient microcapsules composite flame-retardant agent in polymeric matrix material:
The polymeric matrix material can selected from low density polyethylene (LDPE), high density polyethylene (HDPE), polypropylene, polyvinyl chloride,
One of poly 1-butene, polycarbonate, ethylene-vinyl acetate copolymer, polyesters or polystyrene.
The lubricant can be in stearic acid, calcium stearate, butyl stearate, oleamide, microcrystalline wax or white oil
One kind.
The plasticizer can be selected from trioctyl trimellitate (TOTM), dioctyl phthalate, dibutyl phthalate, neighbour
One of phthalic acid dinonyl or diisooctyl phthalate.
The antioxidant can be selected from four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, 2,6-
One of di-tert-butylphenol, bisphenol-A or three (1,4- and tert-butyl-phenyl) phosphorous esters.
The filler can be selected from calcium carbonate, clay, talcum, diatomite, silica, mica powder, asbestos, metal oxygen
One of compound or cellulose powder.
The beneficial effects of the present invention are: II type ammonium polyphosphate is absorbed into flower ball-shaped by microcapsules composite flame-retardant agent of the present invention
In gap on basic magnesium carbonate microballoon.Basic magnesium carbonate belongs to inorganic fire retardants, can be released when heated water vapour and
Carbon dioxide absorbs the oxygen concentration around a large amount of heat and dilution basis material, flame retarding efficiency with higher.The poly- phosphorus of II type
Sour ammonium belongs to a kind of novel expansion type flame retardant, can be used as " acid source " and " gas source ", can be at high temperature in polymer matrix
Body material surface forms the carbon-coating for stablizing densification, plays the role of heat-insulated oxygen-impermeable.It is discharged with flame retarding efficiency height, without noxious material
The features such as.The two is used in combination, its synergistic effect is played, when polymeric matrix material is heated, first basic magnesium carbonate in
The decomposition for starting the first stage in 100~360 DEG C or so ranges, releases vapor, by the II type polyphosphoric acid in bouquet gap
Ammonium releases, and ammonium polyphosphate starts to decompose in 280-300 DEG C or so, and micron-sized II type ammonium polyphosphate disperses more uniform resistance
It fires more efficient.
Melamine formaldehyde resin has nitrogen-atoms abundant, can be used as " gas source ".Melamine-first at high temperature
Urea formaldehyde can release non-ignitable nitrogen and carbon dioxide gas, dilute the air of surrounding.With gas producing efficiency height, do not generate
The features such as toxic gas.To adsorb the flower ball-shaped basic magnesium carbonate of II type ammonium polyphosphate using melamine formaldehyde resin into
Row cladding, the water resistance for improving II type ammonium polyphosphate, the compatibility with basis material, while the nitrogen of flame-retardant system can also be improved
Content, it is swollen that a large amount of non-flammable gases of release can be such that the carbon-coating for stablizing densification caused by the effect of II type ammonium polyphosphate generates
It is swollen, increase the thickness of carbon-coating, heat insulation replacement flame retarding efficiency further enhances.
Although ammonium polyphosphate also with microcapsule coated ammonium polyphosphate modifying, is first utilized flower ball-shaped by the present invention
Basic magnesium carbonate is adsorbed, the compounding ingredients of acquired special construction as core material recycle melamine formaldehyde resin into
Row cladding, flame retarding efficiency are higher.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
(1) it is down to room temperature again after dissolving 10gII type ammonium polyphosphate in 100mL water at 90 DEG C, is filtered to remove a small amount of
Insoluble matter obtains the II type ammonium polyphosphate aqueous solution of higher concentration；
(2) 10g cetyl trimethylammonium bromide is dissolved at room temperature in 80mL water, 40g bouquet is added under stiring
Shape basic magnesium carbonate, and continue stirring 3 hours, gained suspension is filtered, it is neutrality that filter cake, which is washed with water to filtrate, then by filter cake
It is dried in 90 DEG C, obtains the modified flower ball-shaped basic magnesium carbonate in cationic surfactant surface；
(3) basic magnesium carbonate obtained by step (2) is added slowly with stirring II type ammonium polyphosphate solution obtained by step (1)
In, and be continuously stirred at room temperature 3 hours, gained suspension is filtered, then filter cake is dried in 90 DEG C, has been adsorbed II type
The basic magnesium carbonate of ammonium polyphosphate；
(4) melamine of 7.77g and 15mL37% formalin are dissolved in 50mL water, are increased the temperature at 90 DEG C
Reaction 1.5 hours, during which keeping system pH with the solution of bronsted lowry acids and bases bronsted lowry is 8~9, is down to room temperature after reaction and obtains clarification thoroughly
The prepolymer solution of bright melamine formaldehyde resin；
(5) by the dispersion of basic magnesium carbonate obtained by step (3) and suspension obtained in solvent, under stiring by step (4) institute
It obtains melamine formaldehyde resin performed polymer to be slowly added in obtained suspension, regulation system pH value is 4.5, is slowly heated up
It is reacted 4 hours to 80 DEG C, system is cooled to room temperature filtering after reaction, filter cake is washed with water to filtrate as neutrality, then will
Filter cake in 90 DEG C dry, obtain melamine formaldehyde resin cladding basic magnesium carbonate and ammonium polyphosphate compound combustion adjuvant, i.e., one
The efficient microcapsules composite flame-retardant agent of kind；
(6) by microcapsule flame retardant obtained by step (5) and polymeric matrix and lubricant, plasticizer, antioxidant, filler
It is sufficiently mixed uniformly in ratio shown in 1, table 2 and table 3 with open mill, prepares batten using Screw Extrusion injection molding machine；
(7) by batten limit of utilization oxygen index measurer, radial-boom impact tester, universal testing machine obtained by step (6)
Measure its oxygen index (OI), notch impact strength, tensile strength etc..
Embodiment 2
(1) it is down to room temperature again after dissolving 10gII type ammonium polyphosphate in 200mL water at 90 DEG C, is filtered to remove a small amount of
Insoluble matter obtains the II type ammonium polyphosphate aqueous solution of higher concentration；
(2) 8g polyethyleneimine amine hydrochlorate is dissolved at room temperature in 100mL water, 50g flower ball-shaped alkali is added under stiring
Formula magnesium carbonate, and continue stirring 2 hours, gained suspension is filtered, it is neutrality that filter cake, which is washed with water to filtrate, then by filter cake in 90
DEG C drying, obtains the modified flower ball-shaped basic magnesium carbonate in cationic surfactant surface；
(3) basic magnesium carbonate obtained by step (2) is added slowly with stirring II type ammonium polyphosphate solution obtained by step (1)
In, and be continuously stirred at room temperature 2.5 hours, gained suspension is filtered, then filter cake is dried in 90 DEG C, has been adsorbed II
The basic magnesium carbonate of type ammonium polyphosphate；
(4) melamine of 10.36g and 20mL37% formalin are dissolved in 60mL water, increase the temperature to 90 DEG C
Lower reaction 1.5 hours, during which keeping system pH with the solution of bronsted lowry acids and bases bronsted lowry is 8~9.Room temperature is down to after reaction to be clarified
The prepolymer solution of transparent melamine formaldehyde resin；
(5) by the dispersion of basic magnesium carbonate obtained by step (3) and suspension obtained in solvent, under stiring by step (4) institute
It obtains melamine formaldehyde resin performed polymer to be slowly added in obtained suspension, regulation system pH value is 4.5, is slowly heated up
It is reacted 4 hours to 80 DEG C, system is cooled to room temperature filtering after reaction, filter cake is washed with water to filtrate as neutrality.Again will
Filter cake is dried in 90 DEG C.Obtain melamine formaldehyde resin cladding basic magnesium carbonate and ammonium polyphosphate compound combustion adjuvant, i.e., one
The efficient microcapsules composite flame-retardant agent of kind；
(6) by microcapsule flame retardant obtained by step (5) and polymeric matrix and lubricant, plasticizer, antioxidant, filler
It is sufficiently mixed uniformly in ratio shown in 1, table 2 and table 3 with open mill, prepares batten using Screw Extrusion injection molding machine；
(7) by batten limit of utilization oxygen index measurer, radial-boom impact tester, universal testing machine obtained by step (6)
Measure its oxygen index (OI), notch impact strength, tensile strength etc..
Embodiment 3
(1) it is first dispersed 10gII type ammonium polyphosphate in 30mL1.5%NaCl aqueous solution at room temperature with dropper, or else
It is disconnected to add 1.5%NaCl aqueous solution 120mL, it is filtered to remove insoluble matter and obtains the II type ammonium polyphosphate aqueous solution of higher concentration；
(2) 8g polyethyleneimine amine hydrochlorate is dissolved at room temperature in 80mL water, 40g flower ball-shaped alkali formula is added under stiring
Magnesium carbonate, and continue stirring 2 hours, gained suspension is filtered, it is neutrality that filter cake, which is washed with water to filtrate, then by filter cake in 90 DEG C
Drying obtains the modified flower ball-shaped basic magnesium carbonate in cationic surfactant surface；
(3) basic magnesium carbonate obtained by step (2) is added slowly with stirring II type ammonium polyphosphate solution obtained by step (1)
In, and be continuously stirred at room temperature 2.5 hours, gained suspension is filtered, then filter cake is dried in 90 DEG C, has been adsorbed II
The basic magnesium carbonate of type ammonium polyphosphate；
(4) melamine of 10.36g and 20mL37% formalin are dissolved in 60mL water, increase the temperature to 90 DEG C
Lower reaction 1.5 hours, during which keeping system pH with the solution of bronsted lowry acids and bases bronsted lowry is 8~9, is down to room temperature after reaction and is clarified
The prepolymer solution of transparent melamine formaldehyde resin；
(5) by the dispersion of basic magnesium carbonate obtained by step (3) and suspension obtained in solvent, under stiring by step (4) institute
It obtains melamine formaldehyde resin performed polymer to be slowly added in obtained suspension, regulation system pH value is 4.5, is slowly heated up
It is reacted 4 hours to 80 DEG C, system is cooled to room temperature filtering after reaction, filter cake is washed with water to filtrate as neutrality, then will
Filter cake in 90 DEG C dry, obtain melamine formaldehyde resin cladding basic magnesium carbonate and ammonium polyphosphate compound combustion adjuvant, i.e., one
The efficient microcapsules composite flame-retardant agent of kind；
(6) by microcapsule flame retardant obtained by step (5) and polymeric matrix and lubricant, plasticizer, antioxidant, filler
It is sufficiently mixed uniformly in ratio shown in 1, table 2 and table 3 with open mill, prepares batten using Screw Extrusion injection molding machine；
(7) by batten limit of utilization oxygen index measurer, radial-boom impact tester, universal testing machine obtained by step (6)
Measure its oxygen index (OI), notch impact strength, tensile strength etc..
Embodiment 4
(1) it is first dispersed 20gII type ammonium polyphosphate in 30mL1.5%NaCl aqueous solution at room temperature with dropper, or else
It is disconnected to add 1.5%NaCl aqueous solution 120mL, be down to room temperature again after dissolving at 90 DEG C, be filtered to remove insoluble matter obtain it is more highly concentrated
The II type ammonium polyphosphate aqueous solution of degree；
(2) 10g dodecyl benzo triazole is dissolved at room temperature in 120mL water, 60g flower ball-shaped is added under stiring
Basic magnesium carbonate, and continue stirring 2 hours, gained suspension is filtered, filter cake be washed with water to filtrate for neutrality, then by filter cake in
90 DEG C of drying obtain the modified flower ball-shaped basic magnesium carbonate in cationic surfactant surface；
(3) basic magnesium carbonate obtained by step (2) is added slowly with stirring II type ammonium polyphosphate solution obtained by step (1)
In, and be continuously stirred at room temperature 2.5 hours, gained suspension is filtered, then filter cake is dried in 90 DEG C, has been adsorbed II
The basic magnesium carbonate of type ammonium polyphosphate；
(4) melamine of 15.54g and 30mL37% formalin are dissolved in 80mL water, increase the temperature to 90 DEG C
Lower reaction 1.5 hours, during which keeping system pH with the solution of bronsted lowry acids and bases bronsted lowry is 8~9, is down to room temperature after reaction and is clarified
The prepolymer solution of transparent melamine formaldehyde resin；
(5) by the dispersion of basic magnesium carbonate obtained by step (3) and suspension obtained in solvent, under stiring by step (4) institute
It obtains melamine formaldehyde resin performed polymer to be slowly added in obtained suspension, regulation system pH value is 4.5, is slowly heated up
It is reacted 4 hours to 80 DEG C, system is cooled to room temperature filtering after reaction, filter cake is washed with water to filtrate as neutrality.Again will
Filter cake in 90 DEG C dry, obtain melamine formaldehyde resin cladding basic magnesium carbonate and ammonium polyphosphate compound combustion adjuvant, i.e., one
The efficient microcapsules composite flame-retardant agent of kind；
(6) by microcapsule flame retardant obtained by step (5) and polymeric matrix and lubricant, plasticizer, antioxidant, filler
It is sufficiently mixed uniformly in ratio shown in table 1, table 2 and table 3 with open mill, prepares batten using Screw Extrusion injection molding machine；
(7) by batten limit of utilization oxygen index measurer, radial-boom impact tester, universal testing machine obtained by step (6)
Measure its oxygen index (OI), notch impact strength, tensile strength etc..
Application of the 1 embodiment 1-4 microcapsules composite flame-retardant agent of table in PVC
Application of the 2 embodiment 1-4 microcapsules composite flame-retardant agent of table in EVA
Application of the 3 embodiment 1-4 microcapsules composite flame-retardant agent of table in PP
The batten that the microcapsules composite flame-retardant agent of embodiment 1-4 preparation is prepared in different polymeric matrix materials carries out pole
The results are shown in Table 4 for limited oxygen index, tensile strength and impact strength test.
The performance of 4 microcapsules composite fire retardant polymer material of table
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of preparation of efficient microcapsules composite flame-retardant agent, which comprises the following steps:
(1) the II type ammonium polyphosphate of certain mass number is dissolved in the water at high temperature and is down to room temperature again or dissolves at room temperature
In the NaCl aqueous solution that mass fraction is 0.5%~2%, it is filtered to remove a small amount of insoluble matter and obtains the II type polyphosphoric acid of high concentration
Aqueous ammonium；
(2) cationic surfactant is dissolved in the water at room temperature, flower ball-shaped basic magnesium carbonate is added under stiring, and continue
Stirring 1~5 hour, gained suspension is filtered, and it is neutrality that filter cake, which is washed with water to filtrate, then filter cake is dried in 80~120 DEG C,
Obtain the modified flower ball-shaped basic magnesium carbonate in cationic surfactant surface；
(3) basic magnesium carbonate obtained by step (2) is added slowly with stirring in II type ammonium polyphosphate solution obtained by step (1),
And be continuously stirred at room temperature 1~5 hour, gained suspension is filtered, then filter cake is dried in 80~120 DEG C, is adsorbed
The basic magnesium carbonate of II type ammonium polyphosphate；
(4) melamine and 37% formalin are dissolved in the water, increase the temperature at 60~95 DEG C and reacts 0.5-3 hours,
It is 8~10 that the solution of period bronsted lowry acids and bases bronsted lowry, which keeps system pH, is down to room temperature after reaction and obtains the melamine of clear
The prepolymer solution of amine-formaldehyde resin；
(5) it disperses basic magnesium carbonate obtained by step (3) in solvent and suspension is made, it under stiring will be three obtained by step (4)
Paracyanogen amine-formaldehyde resin performed polymer is slowly added in obtained suspension, and regulation system pH value is 3~6, is to slowly warm up to 60
~90 DEG C are reacted 2~8 hours, and system is cooled to room temperature filtering after reaction, and filter cake is washed with water to filtrate as neutrality, then
By filter cake in 80~120 DEG C dry, obtain melamine formaldehyde resin cladding basic magnesium carbonate and ammonium polyphosphate it is compound combustion-supporting
Agent, i.e., a kind of efficient microcapsules composite flame-retardant agent；
(6) by microcapsule flame retardant obtained by step (5) and polymeric matrix and lubricant, plasticizer, antioxidant, filler and its
He is sufficiently mixed uniformly auxiliary agent with open mill, prepares batten using Screw Extrusion injection molding machine；
(7) batten limit of utilization oxygen index measurer, radial-boom impact tester obtained by step (6), universal testing machine are measured
Its oxygen index (OI), notch impact strength, tensile strength etc..
2. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: the step (1),
(2), in (4) raw material mass fraction are as follows: 10~20 parts of II type ammonium polyphosphate, in step (1) water or mass fraction be 0.5%~
80~180 parts of 2% NaCl aqueous solution, 5~20 parts of cationic surfactant, 60~120 parts of water in step (2), alkali formula carbon
30~80 parts of sour magnesium, 5~20 parts of melamine, 37% 5~30 parts of formaldehyde.
3. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, which is characterized in that in the step (6)
The mass fraction of raw material are as follows: 15~40 parts of microcapsules composite flame-retardant agent, 30~50 parts of polymeric matrix material, lubricant 0.1~3
Part, 10~30 parts of toughener, 5~30 parts of filler.
4. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: step (2) sun
Ionic surface active agent be selected from the quaternary ammonium salts sun such as cetyl trimethylammonium bromide, dodecyl benzyl dimethyl ammonium chloride from
The heterocyclics sun such as sub- surfactant, cetyl pyridinium bromide, dodecyl benzo triazole cationic surfactant from
One or more of amine salts cationic surfactants such as sub- surfactant, Suo Luoming A, polyethyleneimine amine hydrochlorate.
5. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: the lubricant is selected from
One of stearic acid, calcium stearate, butyl stearate, oleamide, microcrystalline wax or white oil.
6. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: the plasticizer is selected from
Trioctyl trimellitate (TOTM), dioctyl phthalate, dibutyl phthalate, diisononyl phthalate or O-phthalic
One of sour diisodecyl ester.
7. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: the antioxidant is selected from
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, 2,6- di-tert-butylphenol, bisphenol-A or three (1,4- and
One of tert-butyl-phenyl) phosphorous ester.
8. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: the filler can be with
One in calcium carbonate, clay, talcum, diatomite, silica, mica powder, asbestos, metal oxide or cellulose powder
Kind.
9. the preparation of efficient microcapsules composite flame-retardant agent according to claim 1, it is characterised in that: the polymeric matrix
Material is selected from low density polyethylene (LDPE), high density polyethylene (HDPE), polypropylene, polyvinyl chloride, poly 1-butene, polycarbonate, ethyl vinyl acetate
One of ethylene copolymer, polyesters or polystyrene.
10. a kind of preparation of efficient microcapsules composite flame-retardant agent as claimed in claims 1-9, it is characterised in that: the present invention is also
Provide application of the above-mentioned efficient microcapsules composite flame-retardant agent in polymeric matrix material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040716A (en) * | 2019-12-25 | 2020-04-21 | 江苏晟宏生态纺织科技有限公司 | Preparation method and application of phosphorus-containing flame-retardant polyurethane adhesive |
| CN114315225A (en) * | 2021-12-10 | 2022-04-12 | 千年舟新材科技集团股份有限公司 | Preparation method of flame-retardant shaving board modified based on double-layer coated ammonium polyphosphate microcapsules |
| CN114369334A (en) * | 2022-01-11 | 2022-04-19 | 广东和润新材料股份有限公司 | Preparation method of novel phosphorus-nitrogen flame retardant |
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| CN114369334A (en) * | 2022-01-11 | 2022-04-19 | 广东和润新材料股份有限公司 | Preparation method of novel phosphorus-nitrogen flame retardant |
| CN114369334B (en) * | 2022-01-11 | 2024-01-23 | 广东和润新材料股份有限公司 | Preparation method of phosphorus-nitrogen flame retardant |
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