CN109705396A - A kind of magnesium hydroxide composite fire retardant and preparation method thereof for polyamide - Google Patents
A kind of magnesium hydroxide composite fire retardant and preparation method thereof for polyamide Download PDFInfo
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- CN109705396A CN109705396A CN201811501008.0A CN201811501008A CN109705396A CN 109705396 A CN109705396 A CN 109705396A CN 201811501008 A CN201811501008 A CN 201811501008A CN 109705396 A CN109705396 A CN 109705396A
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- polyamide
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Abstract
The present invention discloses a kind of magnesium hydroxide composite fire retardant and preparation method thereof for polyamide.Magnesium hydroxide composite fire retardant of the present invention for polyamide includes magnesium hydroxide, ammonium polyphosphate, zinc borate and lanthanum nitrate, their mass fraction is respectively 82% ~ 90%, 5% ~ 10%, 2% ~ 5% and 1% ~ 3%.Preparation method of the present invention for the magnesium hydroxide composite fire retardant of polyamide uses water-soluble magnesium salt, aqueous slkali, ammonium polyphosphate, zinc borate and lanthanum nitrate for raw material, successively the following steps are included: water-soluble magnesium salt is configured to aqueous solution by (1)；(2) it disperses powdered ammonium polyphosphate, zinc borate and lanthanum nitrate in magnesium salt solution；(3) aqueous slkali addition is dispersed in the magnesium salt solution of ammonium polyphosphate, zinc borate and lanthanum nitrate powder；(4) polyamide magnesium hydroxide composite fire retardant is made by chemically reacting.Composite flame-retardant agent of the present invention is low in cost, and preparation method is simple, the excellent effect fire-retardant to polyamide.
Description
Technical field
The invention belongs to high molecular material flame retardant area, be related to a kind of fire retardant and preparation method thereof, in particular to it is a kind of
Magnesium hydroxide composite fire retardant and preparation method thereof for polyamide.
Background technique
Polyamide is important engineering plastics, mechanical property, rub resistance, heat resistance, electrical insulating property and excellent weather resistance and hard
It is different, it is widely used in industries such as communications and transportation, electronics, machinery, machinery and packing films.But polyamide is easy burning, because
The fire-retardant of this polyamide has important industrial value.Currently, halogenated flame retardant is the fire-retardant middle maximum resistance of usage amount of polyamide
Agent kind is fired, the high-effect of Environmental Safety is developed in the continuous improvement however as people to own health and environmental protection consciousness
Halogen based flame retardant is the emphasis direction of polyamide flame retardant area.Inorganic fire retardants is with environmentally friendly, smoke amount is low, flame retardant effect is held
It waits so long advantage, receives significant attention, but inorganic fire retardants product is not usually high to the flame retarding efficiency of polyamide at present, to reach
Often additive amount is very big (mass fraction is often beyond 45%) for satisfied flame retardant effect, so that the power of flame-retardant polyamide composite material
Performance is not high, and products application is limited to.
Summary of the invention
The purpose of the present invention is to provide a kind of low in cost, preparation methods simply, excellent to polyamide flame retardant effect
Composite flame-retardant agent and preparation method thereof.
The technical solution for realizing the aim of the invention is as follows: a kind of magnesium hydroxide composite fire retardant for polyamide is
A kind of composite flame-retardant agent comprising magnesium hydroxide, ammonium polyphosphate, zinc borate and lanthanum nitrate.
The present invention is in the magnesium hydroxide composite fire retardant of polyamide, the mass fraction of magnesium hydroxide to be 82% ~ 90%, poly-
The mass fraction of ammonium phosphate is 5% ~ 10%, and the mass fraction of zinc borate is 2% ~ 5%, and the mass fraction of lanthanum nitrate is 1% ~ 3%.
The present invention for polyamide magnesium hydroxide composite fire retardant preparation method, using water-soluble magnesium salt, aqueous slkali,
Ammonium polyphosphate, zinc borate and lanthanum nitrate be raw material, successively the following steps are included:
(1) water-soluble magnesium salt is configured to aqueous solution；
(2) it disperses powdered ammonium polyphosphate, zinc borate and lanthanum nitrate in magnesium salt solution；
(3) aqueous slkali addition is dispersed in the magnesium salt solution of ammonium polyphosphate, zinc borate and lanthanum nitrate；
(4) polyamide magnesium hydroxide composite fire retardant is made by chemically reacting.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, (4) step or the
(3), the system temperature control of (4) step is preferred between 20 ~ 90 DEG C.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, (4) step or the
(3), the reaction time of (4) step was preferred with 1 ~ 10 hour.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, the water-soluble magnesium salt can be with
For the one or more of magnesium chloride, magnesium nitrate or magnesium sulfate；The aqueous slkali can for sodium hydrate aqueous solution, ammonium hydroxide or
The one or more of potassium hydroxide aqueous solution.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, the magnesium that (1) step is prepared
Saline solution concentration is advisable with 0.03 ~ 4.0 mol/L；The concentration of the aqueous slkali is advisable with 0.05 ~ 6.0 mol/L.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, used magnesium salts, poly- phosphorus
Relative mass dosage between sour ammonium, zinc borate and lanthanum nitrate are as follows: the mass fraction of the magnesium hydroxide of magnesium salts conversion is 82 ~ 90
Part, the mass fraction of ammonium polyphosphate is 5 ~ 10 parts, and the mass fraction of zinc borate is 2 ~ 5 parts, and the mass fraction of lanthanum nitrate is 1 ~ 3
Part.
Compared with prior art, the present invention has following remarkable advantage: (1) present invention uses cheap magnesium hydroxide
Based on, it is low in cost；(2) the fire-retardant promotor assembled using ammonium polyphosphate, zinc borate and lanthanum nitrate, prepared compound resistance
Combustion agent is significantly better than prior art products to the flame-retarded efficiency of polyamide；(3) preparation method of the present invention is simple, high production efficiency,
Process costs are low.
Specific embodiment
The present invention for polyamide magnesium hydroxide composite fire retardant be comprising magnesium hydroxide, ammonium polyphosphate, zinc borate and
The composite flame-retardant agent of lanthanum nitrate.
The present invention is in the magnesium hydroxide composite fire retardant of polyamide, the mass fraction of magnesium hydroxide to be 82% ~ 90%, poly-
The mass fraction of ammonium phosphate is 5% ~ 10%, and the mass fraction of zinc borate is 2% ~ 5%, and the mass fraction of lanthanum nitrate is 1% ~ 3%.
The present invention for polyamide magnesium hydroxide composite fire retardant preparation method, using water-soluble magnesium salt, aqueous slkali,
Ammonium polyphosphate, zinc borate and lanthanum nitrate be raw material, successively the following steps are included:
(1) water-soluble magnesium salt is configured to aqueous solution；
(2) it disperses powdered ammonium polyphosphate, zinc borate and lanthanum nitrate in magnesium salt solution；
(3) aqueous slkali addition is dispersed in the magnesium salt solution of ammonium polyphosphate, zinc borate and lanthanum nitrate；
(4) polyamide magnesium hydroxide composite fire retardant is made by chemically reacting.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, (4) step or the
(3), the system temperature of (4) step can be preferred between 20 ~ 90 DEG C in room temperature with control.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, (4) step or the
(3), the reaction time of (4) step was preferred with 1 ~ 10 hour.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, the water-soluble magnesium salt can be with
It is the one or more of magnesium chloride, magnesium nitrate or magnesium sulfate；The aqueous slkali can be sodium hydrate aqueous solution, ammonium hydroxide or
The one or more of potassium hydroxide aqueous solution.The aqueous slkali is preferably sodium hydrate aqueous solution.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, the magnesium that (1) step is prepared
Saline solution concentration is advisable with 0.03 ~ 4.0 mol/L；The concentration of the aqueous slkali is advisable with 0.05 ~ 6.0 mol/L.Aqueous slkali
The hydroxide ion molal quantity that can be contributed is preferably 2 times or 2 times or more of magnesium ion molal quantity contained by magnesium salt solution,
Magnesium ions all in this way can react generation magnesium hydroxide substantially.
It is used for the preparation method of the magnesium hydroxide composite fire retardant of polyamide for the present invention, can be added in reflection system
Suitable pluronic polymer, such as polyethylene glycol, polyvinyl alcohol, can also be added suitable surfactant, to control reaction
The composite flame-retardant agent graininess of generation, and realize that surface is modified.
Preparation method for the present invention for the magnesium hydroxide composite fire retardant of polyamide, used magnesium salts, poly- phosphorus
Relative mass dosage between sour ammonium, zinc borate and lanthanum nitrate are as follows: the mass fraction of the magnesium hydroxide of magnesium salts conversion is 82 ~ 90
Part, the mass fraction of ammonium polyphosphate is 5 ~ 10 parts, and the mass fraction of zinc borate is 2 ~ 5 parts, and the mass fraction of lanthanum nitrate is 1 ~ 3
Part.
Embodiment 1
By the Mg (OH) of 8.5 kg partial size, 200 nm2Powder, 0.6 kg ammonium polyphosphate (molecular weight 1000) powder, 0.3 kg boric acid
Zinc powder and 0.2 kg lanthanum nitrate powder uniformly mix, and obtain magnesium hydroxide composite fire retardant of the present invention.Using the composite flame-proof
6 composite material of Flameproof polyamide is made by melt blending in agent, and when which is 38%, flame retardant rating is
It can reach V-0 grades (3.2mm).
Embodiment 2
By 10.2 kg MgCl2·6H2O solid, which is dissolved in 100L water, is made into MgCl2Solution, then by 0.3 kg ammonium polyphosphate powder
Last (molecular weight 1000), 0.12 kg boric acid zinc powder and 0.08 kg lanthanum nitrate powder are dispersed with stirring in MgCl2In solution, then
Under stirrings, 4 kg NaOH are dissolved in the NaOH aqueous solution being made into 100L water and are slowly dropped into, control temperature room temperature extremely
30 DEG C, the reaction was continued in 30 DEG C after having instilled, from being added dropwise NaOH aqueous solution, the reaction time 9 hours.It is filtered, washed and dried
Obtain magnesium hydroxide composite fire retardant of the present invention.It is compound by the obtained Flameproof polyamide 6 of melt blending using the composite flame-retardant agent
Material, when which is 35%, flame retardant rating can reach V-0 grades (3.2mm).
Embodiment 3
By 5.1kg MgCl2·6H2O solid and 3 kg MgSO4It is dissolved in 100L water and is made into magnesium salt solution, then by 0.2 kg
Ammonium polyphosphate powder (molecular weight 1000), 0.1 kg boric acid zinc powder and 0.06 kg lanthanum nitrate powder are dispersed with stirring in magnesium salts water
In solution, then under stirring, 2 kg NaOH and 2.8kg KOH is dissolved in the aqueous slkali being made into 100L water and are slowly dripped
Enter, controls temperature in room temperature to 70 DEG C, the reaction was continued in 70 DEG C after having instilled, from being added dropwise aqueous slkali, the reaction time 3 hours.
It is filtered, washed and dried to obtain magnesium hydroxide composite fire retardant of the present invention.It is made using the composite flame-retardant agent by melt blending
66 composite material of Flameproof polyamide, when which is 37%, flame retardant rating can reach V-0 grades
(3.2mm)。
Embodiment 4
By 5.1kg MgCl2·6H2O solid and 3.7 kg Mg (NO3)2It is dissolved in 100L water and is made into magnesium salt solution, then will
0.25 kg ammonium polyphosphate powder (molecular weight 1000), 0.11kg boric acid zinc powder and 0.09 kg lanthanum nitrate powder be dispersed with stirring in
In magnesium salt solution, then under stirring, 4 kg NaOH are dissolved in the aqueous slkali being made into 100L water and are slowly dropped into, controlled
Temperature processed is in room temperature to 50 DEG C, and the reaction was continued in 50 DEG C after having instilled, from being added dropwise NaOH aqueous solution, the reaction time 8 hours.It crosses
Filter, wash and be dried to obtain magnesium hydroxide composite fire retardant of the present invention.Resistance is made by melt blending using the composite flame-retardant agent
66 composite material of retardant polyamide, when the composite flame-retardant agent mass fraction 36%, flame retardant rating can reach V-0 grades (3.2mm).
Comparative example 1
Using the Mg (OH) of 200 nm of partial size2Powder is used for Flameproof polyamide 6, Flameproof polyamide 6 as made from melt blending
Composite material, Mg (OH)2When fire retardant mass fraction >=48%, flame retardant rating can be only achieved V-0 grades (3.2mm).
Comparative example 2
By 5.1kg MgCl2·6H2O solid and 3.7 kg Mg (NO3)2It is dissolved in 100L water and is made into magnesium salt solution, stirring
Under state, 4 kg NaOH are dissolved in the aqueous slkali being made into 100L water and are slowly dropped into, controlled temperature in room temperature to 50 DEG C, instill
The reaction was continued in 50 DEG C after complete, from being added dropwise NaOH aqueous solution, the reaction time 8 hours.It is filtered, washed and dried to obtain hydroxide
Magnesium fire retardant.Using obtained flame retardant of magnesium hydroxide, 66 composite material of Flameproof polyamide, Mg are made by melt blending
(OH)2When fire retardant mass fraction >=46%, flame retardant rating can be only achieved V-0 grades (3.2mm).
Claims (8)
1. a kind of magnesium hydroxide composite fire retardant for polyamide, it is characterised in that: for comprising magnesium hydroxide, ammonium polyphosphate,
The composite flame-retardant agent of zinc borate and lanthanum nitrate.
2. the magnesium hydroxide composite fire retardant according to claim 1 for polyamide, it is characterised in that: magnesium hydroxide
Mass fraction is 82% ~ 90%, and the mass fraction of ammonium polyphosphate is 5% ~ 10%, and the mass fraction of zinc borate is 2% ~ 5%, lanthanum nitrate
Mass fraction is 1% ~ 3%.
3. a kind of preparation method of the magnesium hydroxide composite fire retardant for polyamide, it is characterised in that: using water-soluble magnesium salt,
Aqueous slkali, ammonium polyphosphate, zinc borate and lanthanum nitrate be raw material, successively the following steps are included:
(1) water-soluble magnesium salt is configured to aqueous solution；
(2) it disperses powdered ammonium polyphosphate, zinc borate and lanthanum nitrate in magnesium salt solution；
(3) aqueous slkali addition is dispersed in the magnesium salt solution of ammonium polyphosphate, zinc borate and lanthanum nitrate；
(4) polyamide magnesium hydroxide composite fire retardant is made by chemically reacting.
4. the preparation method of the magnesium hydroxide composite fire retardant according to claim 3 for polyamide, it is characterised in that:
The system temperature of (4) step or (3), (4) step is controlled at 20 ~ 90 DEG C.
5. the preparation method of the magnesium hydroxide composite fire retardant according to claim 3 or 4 for polyamide, feature exist
In: the reaction time of (4) step or (3), (4) step is 1 ~ 10 hour.
6. according to the preparation method of the described in any item magnesium hydroxide composite fire retardants for polyamide of claim 3 ~ 5,
Be characterized in that: the water-soluble magnesium salt is the one or more of magnesium chloride, magnesium nitrate or magnesium sulfate；The aqueous slkali is hydrogen
The one or more of aqueous solution of sodium oxide, ammonium hydroxide or potassium hydroxide aqueous solution.
7. according to the preparation method of the described in any item magnesium hydroxide composite fire retardants for polyamide of claim 3 ~ 6,
Be characterized in that: the magnesium salt solution concentration that (1) step is prepared is 0.03 ~ 4.0 mol/L；The concentration of the aqueous slkali is 0.05
~6.0 mol/L。
8. according to the preparation method of the described in any item magnesium hydroxide composite fire retardants for polyamide of claim 3 ~ 7,
Be characterized in that: the relative mass dosage between used magnesium salts, ammonium polyphosphate, zinc borate and lanthanum nitrate is, magnesium salts conversion
The mass fraction of magnesium hydroxide is 82 ~ 90 parts, and the mass fraction of ammonium polyphosphate is 5 ~ 10 parts, and the mass fraction of zinc borate is 2 ~ 5
Part, the mass fraction of lanthanum nitrate is 1 ~ 3 part.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811501008.0A CN109705396B (en) | 2018-12-11 | 2018-12-11 | Magnesium hydroxide composite flame retardant for polyamide and preparation method thereof |
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| CN201811501008.0A CN109705396B (en) | 2018-12-11 | 2018-12-11 | Magnesium hydroxide composite flame retardant for polyamide and preparation method thereof |
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| CN109705396A true CN109705396A (en) | 2019-05-03 |
| CN109705396B CN109705396B (en) | 2022-02-18 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2355111A2 (en) * | 2010-01-27 | 2011-08-10 | King Abdulaziz City for Science and Technology | Cross-linked clean flame retardant wire and cable insulation compositions for enhancing mechanical properties and flame retardancy |
| CN102205980A (en) * | 2011-04-07 | 2011-10-05 | 中国科学院青海盐湖研究所 | Method for preparing monodisperse flaky magnesium hydroxide flame retardant |
| CN102491381A (en) * | 2011-12-16 | 2012-06-13 | 江苏艾特克阻燃材料有限公司 | Preparation method for flame retardant magnesium hydroxide |
| CN103289203A (en) * | 2013-06-24 | 2013-09-11 | 苏州新区佳合塑胶有限公司 | Halogen-free flame-retardant PP composite material and preparation method thereof |
| CN103408960A (en) * | 2013-01-25 | 2013-11-27 | 河北大学 | Lanthanum stannate and application of composition of lanthanum stannate and inorganic flame retardant in halogen-containing superpolymer |
| CN106835850A (en) * | 2016-12-30 | 2017-06-13 | 芜湖市哈贝纸业有限公司 | A kind of anti-mildew packing case paper of shock resistance |
-
2018
- 2018-12-11 CN CN201811501008.0A patent/CN109705396B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2355111A2 (en) * | 2010-01-27 | 2011-08-10 | King Abdulaziz City for Science and Technology | Cross-linked clean flame retardant wire and cable insulation compositions for enhancing mechanical properties and flame retardancy |
| CN102205980A (en) * | 2011-04-07 | 2011-10-05 | 中国科学院青海盐湖研究所 | Method for preparing monodisperse flaky magnesium hydroxide flame retardant |
| CN102491381A (en) * | 2011-12-16 | 2012-06-13 | 江苏艾特克阻燃材料有限公司 | Preparation method for flame retardant magnesium hydroxide |
| CN103408960A (en) * | 2013-01-25 | 2013-11-27 | 河北大学 | Lanthanum stannate and application of composition of lanthanum stannate and inorganic flame retardant in halogen-containing superpolymer |
| CN103289203A (en) * | 2013-06-24 | 2013-09-11 | 苏州新区佳合塑胶有限公司 | Halogen-free flame-retardant PP composite material and preparation method thereof |
| CN106835850A (en) * | 2016-12-30 | 2017-06-13 | 芜湖市哈贝纸业有限公司 | A kind of anti-mildew packing case paper of shock resistance |
Non-Patent Citations (1)
| Title |
|---|
| 陈宝书 主编: "《结构阻燃与新技术教程》", 31 August 2017, 西南交通大学出版社 * |
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