CN106674596A - Method for modifying surface of magnesium hydroxide flame retardant - Google Patents

Method for modifying surface of magnesium hydroxide flame retardant Download PDF

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Publication number
CN106674596A
CN106674596A CN201611008360.1A CN201611008360A CN106674596A CN 106674596 A CN106674596 A CN 106674596A CN 201611008360 A CN201611008360 A CN 201611008360A CN 106674596 A CN106674596 A CN 106674596A
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CN
China
Prior art keywords
magnesium hydroxide
flame retardant
modified
magnesium
mixture
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611008360.1A
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Chinese (zh)
Inventor
孙志鹏
冉文生
姜海成
唐国辉
罗倩
马肖楠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Voins Energy Management Technology Co Ltd
Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Research Institute
Original Assignee
Jiangsu Voins Energy Management Technology Co Ltd
Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Voins Energy Management Technology Co Ltd, Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Research Institute filed Critical Jiangsu Voins Energy Management Technology Co Ltd
Priority to CN201611008360.1A priority Critical patent/CN106674596A/en
Publication of CN106674596A publication Critical patent/CN106674596A/en
Pending legal-status Critical Current

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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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/028—Compounds containing only magnesium as metal
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Fireproofing Substances (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a method for modifying the surface of a magnesium hydroxide flame retardant. The method for modifying the surface of the magnesium hydroxide flame retardant comprises the following steps: (1) drying the magnesium hydroxide at low temperature of 4 to 8 DEG C for 2 hours, and performing pulverization after drying at low temperature to obtain magnesium hydroxide powder; (2) dissolving the magnesium hydroxide powder into pure water, stirring at the stirring speed of 200 to 300 rpm/min, adding laurate, metal magnesium and maleic anhydride, performing ultrasonic treatment at the ultrasonic power of 80 to 120 W for 20 to 30 minutes, and performing vacuum drying after ultrasonic treatment to obtain a mixture ; (3) placing the mixture subjected to vacuum drying in the above step into a Co-60 radiation source, performing radiation for one week, packaging, sealing and allowing standing still for 2 weeks. The modification method is simple to operate and low in cost, and the economic benefit is greatly improved ; the compatibility between the modified magnesium hydroxide and a macromolecular material is obviously improved.

Description

A kind of modified method in flame retardant of magnesium hydroxide surface
Technical field
The present invention relates to a kind of material modification field, the modified method in specifically a kind of flame retardant of magnesium hydroxide surface.
Background technology
Magnesium hydroxide is the conventional halogen-free flame retardants of mesh first two, has the advantages that inexpensive, efficient suppression cigarette, in many fields Close, such as electric wire, coated coating etc., be used widely.But due to its surface energy it is higher, with polymer-based compatability Poor, conventional coupling agent etc. is surface-treated to which at present, compatible between magnesium hydroxide and macromolecular material to improve Property.It is high to there is price in coupling agent；Powder body bulk specific weight after surface treatment is low, dust weight；Treatment temperature is high, it usually needs Using inflammable and explosive organic solvent, it is more difficult to operate.Be polymerized using high-molecular in-situ, the height of even compact is formed in powder surface Molecule coating film, can effectively improve magnesium hydroxide and the high molecular compatibility of matrix, and give modified powder body fire retardant with Between other functions feature, such as toughness reinforcing, the different macromolecules of two kinds of increase the features such as the compatibility.In-situ polymerization is using wet at present Method process, will powder body be scattered in water or other solvents, then monomer is polymerized in powder surface, these polymerization processes are usual It is incubated several hours.This processing method there are high energy consumption, post processing it is complicated, it is seriously polluted the problems such as.Chinese patent Shen Number a kind of manufacture method of modified non-halogen fire retardant please be disclosed for 200510112398.9, using in situ poly- in this application file Legal, which passes through non-flame resistant dose is put in the kneader of high shear and is sufficiently stirred for, and is subsequently adding polymerized monomer and initiator, obtains To the modified non-halogen fire retardant of fillibility, the method has and is not required to solvent, and polymerization time is short, the features such as production efficiency is high, obtains Modified flame-retardant agent have bulk density big, fire resistance is good, the features such as concentration is high.But just it is adsorbed in the freedom of powder surface For base monomer, due to the high surface energy of powder surface, the monomer molecule of powder surface is adsorbed in, is had similar to " fixation " in powder The characteristics of body surface face, the molecular motion of these monomers, receive the restriction of powder surface energy, it is difficult to be further polymerized, in free radical Under initiator causes, cause to be wrapped by the liquid layer that thin layer is there are between powder body and covering material, not only monomer conversion is not Material modified mechanical performance that is high and obtaining also is affected, and this method for coating can only partly improve powder body with height The compatibility of molecular material, easily causing material modified have abnormal flavour, the bad phenomenon such as unpolymerized small molecule migration easily occurs.
The content of the invention
It is an object of the invention to provide a kind of modified method in flame retardant of magnesium hydroxide surface, to solve above-mentioned background skill The problem proposed in art.
For achieving the above object, the present invention provides following technical scheme：
A kind of modified method in flame retardant of magnesium hydroxide surface, comprises the following steps：
(1) magnesium hydroxide is carried out into cold drying 2h, cryogenic temperature is 4 DEG C -8 DEG C, is pulverized, obtain after cold drying Magnesium hydroxide powder；
(2) subsequently magnesium hydroxide powder is dissolved in pure water, mixing speed is 200-300rpm/min, is added after stirring Laurate, magnesium metal and maleic anhydride, ultrasonic Treatment, ultrasonic power are 80-120W, and sonication times are 20- 30min, is vacuum dried after ultrasound, is obtained mixture；
(3) mixture after be vacuum dried above-mentioned steps is placed in Co-60 radiation sources and radiates one week, is subsequently wrapped Dress, sealing, standing are obtained final product for 2 weeks.
As further scheme of the invention：The cryogenic temperature is 6 DEG C.
As further scheme of the invention：Mixing speed is 250rpm/min.
As further scheme of the invention：Ultrasonic power is 100W, and sonication times are 25min.
Compared with prior art, the invention has the beneficial effects as follows：
The method of modifying that the present invention is adopted, it is simple to operate, with low cost, substantially increase economic benefit；Modified hydrogen Magnesium oxide fire retardant significantly improves its compatibility between macromolecular material.
Specific embodiment
The technical scheme of this patent is described in more detail with reference to specific embodiment.
Embodiment 1
A kind of modified method in flame retardant of magnesium hydroxide surface, comprises the following steps：
(1) magnesium hydroxide is carried out into cold drying 2h, cryogenic temperature is 4 DEG C, is pulverized, hydrogen-oxygen is obtained after cold drying Change magnesium dust；
(2) subsequently magnesium hydroxide powder is dissolved in pure water, mixing speed is 200rpm/min, and Laurel is added after stirring Acid esters, magnesium metal and maleic anhydride, ultrasonic Treatment, ultrasonic power are 80W, and sonication times are 20min, are carried out after ultrasound Vacuum drying, obtains mixture；
(3) mixture after be vacuum dried above-mentioned steps is placed in Co-60 radiation sources and radiates one week, is subsequently wrapped Dress, sealing, standing are obtained final product for 2 weeks.
The contact angle test data of flame retardant of magnesium hydroxide by obtained in above-mentioned technique is reduced to by 91.52 before modified 35.14。
Embodiment 2
A kind of modified method in flame retardant of magnesium hydroxide surface, comprises the following steps：
(1) magnesium hydroxide is carried out into cold drying 2h, cryogenic temperature is 6 DEG C, is pulverized, hydrogen-oxygen is obtained after cold drying Change magnesium dust；
(2) subsequently magnesium hydroxide powder is dissolved in pure water, mixing speed is 250rpm/min, and Laurel is added after stirring Acid esters, magnesium metal and maleic anhydride, ultrasonic Treatment, ultrasonic power are 100W, and sonication times are 25min, and ultrasound is laggard Row vacuum drying, obtains mixture；
(3) mixture after be vacuum dried above-mentioned steps is placed in Co-60 radiation sources and radiates one week, is subsequently wrapped Dress, sealing, standing are obtained final product for 2 weeks.
The contact angle test data of flame retardant of magnesium hydroxide by obtained in above-mentioned technique is reduced to by 91.52 before modified 30.04。
Embodiment 3
A kind of modified method in flame retardant of magnesium hydroxide surface, comprises the following steps：
(1) magnesium hydroxide is carried out into cold drying 2h, cryogenic temperature is 8 DEG C, is pulverized, hydrogen-oxygen is obtained after cold drying Change magnesium dust；
(2) subsequently magnesium hydroxide powder is dissolved in pure water, mixing speed is 300rpm/min, and Laurel is added after stirring Acid esters, magnesium metal and maleic anhydride, ultrasonic Treatment, ultrasonic power are 120W, and sonication times are 30min, and ultrasound is laggard Row vacuum drying, obtains mixture；
(3) mixture after be vacuum dried above-mentioned steps is placed in Co-60 radiation sources and radiates one week, is subsequently wrapped Dress, sealing, standing are obtained final product for 2 weeks.
The contact angle test data of flame retardant of magnesium hydroxide by obtained in above-mentioned technique is reduced to by 91.52 before modified 31.76。
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped Containing an independent technical scheme, this narrating mode of description is only that those skilled in the art should for clarity Using description as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art Understandable other embodiment.

Claims (4)

1. a kind of method that flame retardant of magnesium hydroxide surface is modified, it is characterised in that comprise the following steps：
(1) magnesium hydroxide is carried out into cold drying 2h, cryogenic temperature is 4 DEG C -8 DEG C, is pulverized, hydrogen-oxygen is obtained after cold drying Change magnesium dust；
(2) subsequently magnesium hydroxide powder is dissolved in pure water, mixing speed is 200-300rpm/min, and Laurel is added after stirring Acid esters, magnesium metal and maleic anhydride, ultrasonic Treatment, ultrasonic power are 80-120W, and sonication times are 20-30min, are surpassed It is vacuum dried after sound, is obtained mixture；
(3) mixture after be vacuum dried above-mentioned steps is placed in Co-60 radiation sources and radiates one week, subsequently carries out packing, close Envelope, standing are obtained final product for 2 weeks.
2. the method that flame retardant of magnesium hydroxide surface according to claim 1 is modified, it is characterised in that the cryogenic temperature For 6 DEG C.
3. the method for the modified method in flame retardant of magnesium hydroxide surface according to claim 1 and 2, it is characterised in that stir Speed is mixed for 250rpm/min.
4. the method for the modified method in flame retardant of magnesium hydroxide surface according to claim 3, it is characterised in that ultrasound wave Power is 100W, and sonication times are 25min.
CN201611008360.1A 2016-11-16 2016-11-16 Method for modifying surface of magnesium hydroxide flame retardant Pending CN106674596A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1358803A (en) * 2000-12-15 2002-07-17 四川大学 Method for surface modifying inorganic particle
CN101974257A (en) * 2010-09-19 2011-02-16 广东宇星锑业有限公司 Method for modifying aluminum hydroxide/magnesium hydroxide flame retardant

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1358803A (en) * 2000-12-15 2002-07-17 四川大学 Method for surface modifying inorganic particle
CN101974257A (en) * 2010-09-19 2011-02-16 广东宇星锑业有限公司 Method for modifying aluminum hydroxide/magnesium hydroxide flame retardant

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
冯钠等: "氢氧化镁表面化学改性及其在塑料中的应用研究进展", 《塑料科技》 *

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Application publication date: 20170517