CN111073055A - Carrier-free magnesium hydroxide flame retardant master batch and preparation method thereof - Google Patents
Carrier-free magnesium hydroxide flame retardant master batch and preparation method thereof Download PDFInfo
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- CN111073055A CN111073055A CN201911340885.9A CN201911340885A CN111073055A CN 111073055 A CN111073055 A CN 111073055A CN 201911340885 A CN201911340885 A CN 201911340885A CN 111073055 A CN111073055 A CN 111073055A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/223—Packed additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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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
- 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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- 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
- C08K9/10—Encapsulated ingredients
Abstract
The invention relates to the technical field of flame retardant synthesis, and particularly discloses a carrier-free magnesium hydroxide flame retardant master batch and a preparation method thereof. The preparation raw materials at least comprise the following components in parts by weight: 95-99 parts of magnesium hydroxide, 0.1-1.5 parts of coupling agent, 0.5-3 parts of surfactant, 40-60 parts of water and 1-3 parts of binder. The preparation method has the advantages of simple preparation process, low cost, great reduction of dust pollution and the like, and the magnesium hydroxide is subjected to surface treatment by adopting the coupling agent and the surfactant, so that the prepared magnesium hydroxide has high surface coating rate, high decomposition temperature and good flame retardant property, and the application field of the magnesium hydroxide flame retardant is effectively improved; in addition, when the flame retardant prepared by the invention is compounded with a high molecular material, the phenomenon that the flame retardant is easy to agglomerate per se is relieved, and the compatibility of the inorganic flame retardant and the high molecular polymer is improved.
Description
Technical Field
The invention relates to the technical field of flame retardant synthesis, in particular to a carrier-free magnesium hydroxide flame retardant master batch and a preparation method thereof.
Background
Magnesium hydroxide has various performances of flame retardance, smoke abatement, dripping resistance, filling and the like, has wide application in the aspects of flame retardance, environmental protection, medicine, ceramics and the like, and is deeply applied to various fields of national economy. With the continuous progress of society, the requirements of people on new materials are continuously improved, the quality index of magnesium hydroxide products not only stays at the original product purity, but also puts higher requirements on the product form and the surface performance.
The magnesium hydroxide flame retardant plays a role in flame retardance by means of chemical decomposition and heat absorption and water release when being heated, so that the magnesium hydroxide flame retardant has the advantages of no toxicity, low smoke, stable chemical property of magnesium oxide generated after decomposition, no secondary pollution and the like. However, the surface of the magnesium hydroxide flame retardant naturally presents the properties of hydrophilic and oleophobic, if the polymer material is filled with magnesium hydroxide powder without surface treatment, the magnesium hydroxide powder is difficult to uniformly disperse in the organic high polymer, and other properties (such as mechanical property, processing property and the like) of the polymer material are seriously deteriorated, so that the magnesium hydroxide must be subjected to surface modification to change the surface property of the natural hydrophilic and oleophobic, improve the compatibility with the polymer, reduce the influence on the processing property and the mechanical property of the polymer product and even improve the properties.
Disclosure of Invention
In order to solve the technical problems, the invention provides a carrier-free magnesium hydroxide flame retardant master batch, which at least comprises the following preparation raw materials in parts by weight: 95-99 parts of magnesium hydroxide, 0.1-1.5 parts of coupling agent, 0.5-3 parts of surfactant, 40-60 parts of water and 1-3 parts of binder.
As a preferred technical scheme, the carrier-free magnesium hydroxide flame retardant master batch at least comprises the following preparation raw materials in parts by weight: 96-98 parts of magnesium hydroxide, 0.5-1.2 parts of coupling agent, 1.5-2.5 parts of surfactant, 45-55 parts of water and 1.5-2.5 parts of binder.
As a preferable technical scheme, the particle size of the magnesium hydroxide is 1-5 μm.
As a preferable technical scheme, the particle size of the magnesium hydroxide is 3 μm.
As a preferable technical scheme, the coupling agent is selected from one or more of aminosilane coupling agent, vinyl silane coupling agent and epoxy silane coupling agent.
As a preferable technical scheme, the coupling agent is a combination of N-aminoethyl-gamma-aminopropyltrimethoxysilane and vinyl tri (2-methoxyethoxy) silane, wherein the mass ratio of the N-aminoethyl-gamma-aminopropyltrimethoxysilane to the vinyl tri (2-methoxyethoxy) silane is 1: (0.5-2.8).
As a preferred technical scheme, the surface active agent is an anionic surface active agent and a nonionic surface active agent.
As a preferable technical scheme, the surfactant is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of the sodium stearate to the isomeric tridecanol polyoxyethylene ether is 1: (0.5-3.5).
As a preferred technical solution, it is proposed that,
the second aspect of the invention provides a preparation method of carrier-free magnesium hydroxide flame retardant master batch, which comprises the following steps: the binder is selected from one or more of polyvinyl butyral, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, PE wax, silicone oil and sodium silicate.
(1) Dissolving a coupling agent in water at 30-50 ℃, and stirring for 10-90min to obtain a solution A;
(2) putting magnesium hydroxide into a high-speed mixer, preheating to 60-90 ℃ at 600r/min, adding the solution A into the magnesium hydroxide in a stirring state, and stirring and modifying for 10-300min at 800-1200 r/min; then adding surfactant, stirring at 60-90 deg.C for 10-360min, screw extruding, and oven drying at 85-100 deg.C.
Has the advantages that: the invention provides a carrier-free magnesium hydroxide flame retardant master batch and a preparation method thereof, the preparation process is simple, the cost is lower, the dust pollution is greatly reduced, and the like, the magnesium hydroxide is subjected to surface treatment by adopting a coupling agent and a surfactant, so that the prepared magnesium hydroxide has high surface coating rate, high decomposition temperature and good flame retardant property, and the application field of the magnesium hydroxide flame retardant is effectively improved; in addition, when the flame retardant prepared by the invention is compounded with a high molecular material, the phenomenon that the flame retardant is easy to agglomerate per se is relieved, and the compatibility of the inorganic flame retardant and the high molecular polymer is improved.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the technical problems, the first aspect of the invention provides an unsupported magnesium hydroxide flame retardant master batch, which at least comprises the following preparation raw materials in parts by weight: 95-99 parts of magnesium hydroxide, 0.1-1.5 parts of coupling agent, 0.5-3 parts of surfactant, 40-60 parts of water and 1-3 parts of binder.
In a preferred embodiment, the carrier-free magnesium hydroxide flame retardant masterbatch provided by the invention is prepared from at least the following raw materials in parts by weight: 96-98 parts of magnesium hydroxide, 0.5-1.2 parts of coupling agent, 1.5-2.5 parts of surfactant, 45-55 parts of water and 1.5-2.5 parts of binder.
In a most preferred embodiment, the carrier-free magnesium hydroxide flame retardant master batch provided by the invention is prepared from at least the following raw materials in parts by weight: 96.5 parts of magnesium hydroxide, 1 part of coupling agent, 2.5 parts of surfactant, 50 parts of water and 2 parts of binder.
Magnesium hydroxide
The magnesium hydroxide of the invention is white amorphous powder. The nickelite, light-burned magnesite and the like are also known as caustic magnesite, and suspension of magnesium hydroxide in water is called magnesium hydroxide emulsion, which is abbreviated as magnesium emulsion; the magnesium hydroxide is colorless hexagonal column crystal or white powder, is insoluble in water and alcohol, is soluble in dilute acid and ammonium salt solution, and has weak alkalinity in water solution. The solubility in water is small, but the water-soluble fraction is completely ionized.
In a preferred embodiment, the magnesium hydroxide according to the invention has a particle size of 1 to 5 μm.
In a most preferred embodiment, the magnesium hydroxide of the present invention has a particle size of 3 μm.
Coupling agent
The coupling agent is a substance containing two functional groups with different properties, and the molecular structure of the coupling agent is mainly characterized in that molecules contain two groups with different chemical properties, one group is an inorganophilic group and is easy to chemically react with the surface of an inorganic substance; the other is an organophilic group which is capable of chemically reacting with or forming hydrogen bonds soluble in synthetic resins or other polymers. Therefore, the coupling agent is called as a molecular bridge and is used for improving the interface action between inorganic matters and organic matters, so that the properties of the composite material, such as physical properties, electrical properties, thermal properties, optical properties and the like, are greatly improved.
In a preferred embodiment, the coupling agent of the present invention is selected from one or more of aminosilane coupling agents, vinylsilane coupling agents, and epoxysilane coupling agents.
As examples of aminosilane coupling agents, there may be mentioned: 3-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, phenylaminomethyltriethoxysilane, phenylaminomethyltrimethoxysilane, aminoethylaminoaminopropyltrimethoxysilane, polyaminoalkyltrialkoxysilane, N-aminoethyl-gamma-aminopropyltrimethoxysilane.
As examples of the vinyl silane coupling agent, there may be mentioned: vinyltrichlorosilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (2-methoxyethoxy) silane, vinyltriacetoxysilane, vinyltributylsilane triperoxide, vinylmethyldichlorosilane.
Examples of the epoxysilane coupling agent include gamma- (2, 3-epoxypropyl) propyltrimethoxysilane, gamma- (2, 3-epoxypropyl) propyltriethoxysilane, gamma- (β -aminoethyl) aminopropyltrimethoxysilane, gamma- (β -aminoethyl) aminopropyltrimethoxysilane, gamma-ureidopropyltriethoxysilane, and anilinomethyltrimethoxysilane.
In a preferred embodiment, the coupling agent of the present invention is a combination of N-aminoethyl- γ -aminopropyltrimethoxysilane and vinyltris (2-methoxyethoxy) silane, wherein the mass ratio of N-aminoethyl- γ -aminopropyltrimethoxysilane to vinyltris (2-methoxyethoxy) silane is 1: (0.5-2.8).
In a more preferred embodiment, the coupling agent of the present invention is a combination of N-aminoethyl- γ -aminopropyltrimethoxysilane and vinyltris (2-methoxyethoxy) silane, wherein the mass ratio of N-aminoethyl- γ -aminopropyltrimethoxysilane to vinyltris (2-methoxyethoxy) silane is 1: (1-2).
In a most preferred embodiment, the coupling agent of the present invention is a combination of N-aminoethyl- γ -aminopropyltrimethoxysilane and vinyltris (2-methoxyethoxy) silane, wherein the mass ratio of N-aminoethyl- γ -aminopropyltrimethoxysilane to vinyltris (2-methoxyethoxy) silane is 1: 1.5.
the CAS number of the N-aminoethyl-gamma-aminopropyltrimethoxysilane is 1760-24-3.
The CAS number of the vinyltris (2-methoxyethoxy) silane of the present invention is 1067-53-4.
Surface active agent
The surfactant is a substance which is added in a small amount and can cause the interface state of a solution system of the surfactant to change obviously. Has fixed hydrophilic and lipophilic groups and can be directionally arranged on the surface of the solution. The molecular structure of the surfactant has amphipathy: one end is a hydrophilic group, and the other end is a hydrophobic group; the hydrophilic group is often a polar group, such as carboxylic acid, sulfonic acid, sulfuric acid, amino or amino groups and salts thereof, hydroxyl, amide, ether linkages, and the like may also be used as the polar hydrophilic group; and the hydrophobic group is often a non-polar hydrocarbon chain, such as a hydrocarbon chain of 8 or more carbon atoms.
In a preferred embodiment, the surfactants of the present invention are anionic surfactants and nonionic surfactants.
As examples of the anionic surfactant, there may be enumerated: sodium stearate, zinc stearate, calcium stearate, magnesium stearate, sodium fatty acid, sodium lauryl polyoxyethylene ether sulfate, sodium fatty alcohol polyoxyethylene ether carboxylate, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate.
As examples of the nonionic surfactant, there can be cited: isomeric dodecyl alcohol polyoxyethylene ether, isomeric tridecyl alcohol polyoxyethylene ether, isooctyl alcohol polyoxyethylene ether, octyl alcohol tri-polyoxyethylene ether, dodecyl alcohol hexa-polyoxyethylene ether, tridecyl alcohol deca-polyoxyethylene ether, pentadecyl alcohol hexa-polyoxyethylene ether, hexadecyl alcohol octa-polyoxyethylene ether, undecyl alcohol hexa-polyoxyethylene ether, dodecyl alcohol deca-polyoxyethylene ether, oleyl alcohol polyoxyethylene ether, polyoxyethylene alkylolamide and polyoxyethylene sorbitan monooleate. Sorbitan fatty acid ester, sorbitan monostearate, sorbitan monooleate polyoxyethylene ether, polyoxyethylene sorbitan monostearate, fatty alcohol ether phosphate, alkylphenol polyoxyethylene, coconut oil fatty acid diethanolamide, polyoxyethylene polyoxypropylene oleate ester of oleic acid, isomeric alcohol polyoxyethylene ether, triethanolamine oleate soap, alkylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether.
The CAS number of the isomeric tridecanol polyoxyethylene ether is 9043-30-5.
In a preferred embodiment, the surfactant of the present invention is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of sodium stearate to isomeric tridecanol polyoxyethylene ether is 1: (0.5-3.5).
In a more preferred embodiment, the surfactant of the present invention is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of sodium stearate to isomeric tridecanol polyoxyethylene ether is 1: (0.5-3.5).
In a most preferred embodiment, the surfactant of the present invention is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of sodium stearate to isomeric tridecanol polyoxyethylene ether is 1: 2.
binder
In a preferred embodiment, the binder according to the invention is selected from one or more of polyvinyl butyral, nitrocellulose, polyvinyl alcohol, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, PE wax, silicone oil, sodium silicate.
In a most preferred embodiment, the binder of the present invention is a PE wax.
In experiments, the inventor of the application finds that magnesium hydroxide is subjected to surface modification treatment by firstly adopting a silane coupling agent containing amino and vinyl, and then adopting sodium stearate and isomeric tridecanol polyoxyethylene ether as a surfactant, so that the surface of the magnesium hydroxide treated by the silane coupling agent is more hydrophobic and oleophilic, and the probability of the modified magnesium hydroxide being granular is improved. The inventor speculates that the sodium stearate and the isomeric tridecanol polyoxyethylene ether contain long carbon chains, are easy to wind into a network structure to cover more magnesium hydroxide, so that the modified magnesium hydroxide is difficult to dust. In addition, when the modified magnesium hydroxide is used for a high polymer resin material and used as a flame retardant filler, the compatibility of the magnesium hydroxide in a high polymer system can be improved, and the mechanical property of the high polymer material, especially a polypropylene material, can be effectively improved.
The second aspect of the invention provides a preparation method of carrier-free magnesium hydroxide flame retardant master batch, which comprises the following steps:
(1) dissolving a coupling agent in water at 30-50 ℃, and stirring for 10-90min to obtain a solution A;
(2) putting magnesium hydroxide into a high-speed mixer, preheating to 60-90 ℃ at 600r/min, adding the solution A into the magnesium hydroxide in a stirring state, and stirring and modifying for 10-300min at 800-1200 r/min; then adding surfactant, stirring at 60-90 deg.C for 10-360min, screw extruding, and oven drying at 85-100 deg.C.
Examples
Example 1
Embodiment 1 provides a carrier-free magnesium hydroxide flame retardant master batch, which comprises, by weight, 96.5 parts of magnesium hydroxide, 1 part of a coupling agent, 2.5 parts of a surfactant, 50 parts of water and 2 parts of a binder.
The particle size of the magnesium hydroxide is 3 mu m.
The coupling agent is a combination of N-aminoethyl-gamma-aminopropyltrimethoxysilane and vinyl tri (2-methoxyethoxy) silane, wherein the mass ratio of the N-aminoethyl-gamma-aminopropyltrimethoxysilane to the vinyl tri (2-methoxyethoxy) silane is 1: 1.5.
the surfactant is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of the sodium stearate to the isomeric tridecanol polyoxyethylene ether is 1: 2.
the binder is PE wax.
The preparation method of the carrier-free magnesium hydroxide flame retardant master batch comprises the following steps:
(1) dissolving a coupling agent in water at 40 ℃, and stirring for 60min to obtain a solution A;
(2) putting magnesium hydroxide into a high-speed mixer, preheating to 70 ℃ at 600r/min, adding the solution A into the magnesium hydroxide in a stirring state, and stirring and modifying for 210min at 1000 r/min; then adding surfactant, stirring at 80 deg.C for 300min, screw extruding, and oven drying at 90 deg.C.
Example 2
Embodiment 2 provides a carrier-free magnesium hydroxide flame retardant master batch, which comprises, by weight, 95 parts of magnesium hydroxide, 0.1 part of a coupling agent, 0.5 part of a surfactant, 40 parts of water and 1 part of a binder. .
The particle size of the magnesium hydroxide is 3 mu m.
The coupling agent is a combination of N-aminoethyl-gamma-aminopropyltrimethoxysilane and vinyl tri (2-methoxyethoxy) silane, wherein the mass ratio of the N-aminoethyl-gamma-aminopropyltrimethoxysilane to the vinyl tri (2-methoxyethoxy) silane is 1: 1.5.
the surfactant is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of the sodium stearate to the isomeric tridecanol polyoxyethylene ether is 1: 2.
the binder is PE wax.
The preparation method of the carrier-free magnesium hydroxide flame retardant master batch comprises the following steps:
(1) dissolving a coupling agent in water at 40 ℃, and stirring for 60min to obtain a solution A;
(2) putting magnesium hydroxide into a high-speed mixer, preheating to 70 ℃ at 600r/min, adding the solution A into the magnesium hydroxide in a stirring state, and stirring and modifying for 210min at 1000 r/min; then adding surfactant, stirring at 80 deg.C for 300min, screw extruding, and oven drying at 90 deg.C.
Example 3
Embodiment 3 provides a carrier-free magnesium hydroxide flame retardant master batch, which comprises, by weight, 99 parts of magnesium hydroxide, 1.5 parts of a coupling agent, 3 parts of a surfactant, 60 parts of water and 2.5 parts of a binder.
The particle size of the magnesium hydroxide is 3 mu m.
The coupling agent is a combination of N-aminoethyl-gamma-aminopropyltrimethoxysilane and vinyl tri (2-methoxyethoxy) silane, wherein the mass ratio of the N-aminoethyl-gamma-aminopropyltrimethoxysilane to the vinyl tri (2-methoxyethoxy) silane is 1: 1.5.
the surfactant is a combination of sodium stearate and isomeric tridecanol polyoxyethylene ether, wherein the mass ratio of the sodium stearate to the isomeric tridecanol polyoxyethylene ether is 1: 2.
the binder is PE wax.
The preparation method of the carrier-free magnesium hydroxide flame retardant master batch comprises the following steps:
(1) dissolving a coupling agent in water at 40 ℃, and stirring for 60min to obtain a solution A;
(2) putting magnesium hydroxide into a high-speed mixer, preheating to 70 ℃ at 600r/min, adding the solution A into the magnesium hydroxide in a stirring state, and stirring and modifying for 210min at 1000 r/min; then adding surfactant, stirring at 80 deg.C for 300min, screw extruding, and oven drying at 90 deg.C.
Example 4
Example 4 is similar to example 1 except that the coupling agent is N-aminoethyl-gamma-aminopropyltrimethoxysilane.
Example 5
Example 5 is similar to example 1 except that the coupling agent is vinyltris (2-methoxyethoxy) silane.
Example 6
Example 6 is similar to example 1 except that the surfactant is sodium stearate.
Example 7
Example 7 is similar to example 1 except that the surfactant is isomeric tridecanol polyoxyethylene ether.
Evaluation of Performance
Activation index: grinding the carrier-free magnesium hydroxide flame retardant master batches prepared in the embodiments 1 to 7 into powder, respectively adding 10g of the powder into a beaker, then adding 150mL of distilled water into the beaker, stirring for 2min, standing for 1h, separating the material precipitated at the bottom of the beaker, drying, cooling and weighing. The activation index was calculated according to the following formula, and the data results are shown in table 1 below.
H (activation index) ═ m (mass of sample floated)/m (total mass of sample) × 100%
TABLE 1 activation index
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Index of activation | 99.3％ | 95％ | 97％ | 85％ |
| Example 5 | Example 6 | Example 7 | ||
| Index of activation | 87％ | 86％ | 83％ |
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The carrier-free magnesium hydroxide flame retardant master batch is characterized by at least comprising the following preparation raw materials in parts by weight: 95-99 parts of magnesium hydroxide, 0.1-1.5 parts of coupling agent, 0.5-3 parts of surfactant, 40-60 parts of water and 1-3 parts of binder.
2. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 1, wherein the unsupported magnesium hydroxide flame retardant masterbatch is prepared from at least the following raw materials in parts by weight: 96-98 parts of magnesium hydroxide, 0.5-1.2 parts of coupling agent, 1.5-2.5 parts of surfactant, 45-55 parts of water and 1.5-2.5 parts of binder.
3. The unsupported magnesium hydroxide flame-retardant masterbatch according to claim 1, wherein the particle size of the magnesium hydroxide is 1 to 5 μm.
4. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 3, wherein the particle size of the magnesium hydroxide is 3 μm.
5. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 1, wherein the coupling agent is selected from one or more of an aminosilane coupling agent, a vinylsilane coupling agent, and an epoxysilane coupling agent.
6. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 5, wherein the coupling agent is a combination of N-aminoethyl- γ -aminopropyltrimethoxysilane and vinyltris (2-methoxyethoxy) silane, wherein the mass ratio of N-aminoethyl- γ -aminopropyltrimethoxysilane to vinyltris (2-methoxyethoxy) silane is 1: (0.5-2.8).
7. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 1, wherein the surfactant is an anionic surfactant and a nonionic surfactant.
8. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 7, wherein the surfactant is a combination of sodium stearate and isotridecanol polyoxyethylene ether, wherein the mass ratio of sodium stearate to isotridecanol polyoxyethylene ether is 1: (0.5-3.5).
9. The unsupported magnesium hydroxide flame retardant masterbatch according to claim 1, wherein the binder is selected from one or more of polyvinyl butyral, nitrocellulose, polyvinyl alcohol, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, PE wax, silicone oil, and sodium silicate.
10. The method for preparing the unsupported magnesium hydroxide flame retardant masterbatch according to any one of claims 1 to 9, wherein the method for preparing the unsupported magnesium hydroxide flame retardant masterbatch comprises the following steps:
(1) dissolving a coupling agent in water at 30-50 ℃, and stirring for 10-90min to obtain a solution A;
(2) putting magnesium hydroxide into a high-speed mixer, preheating to 60-90 ℃ at 600r/min, adding the solution A into the magnesium hydroxide in a stirring state, and stirring and modifying for 10-300min at 800-1200 r/min; then adding surfactant, stirring at 60-90 deg.C for 10-360min, screw extruding, and oven drying at 85-100 deg.C.
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Cited By (4)
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|---|---|---|---|---|
| CN112266536A (en) * | 2020-11-05 | 2021-01-26 | 广东天雄新材料科技股份有限公司 | Carrier-free weather-resistant PP flame-retardant master batch and preparation method and application thereof |
| CN112724465A (en) * | 2020-12-29 | 2021-04-30 | 宁波艾克姆新材料有限公司 | Flame-retardant silane crosslinked nano modified polyolefin pre-dispersed master batch auxiliary |
| CN114426702A (en) * | 2022-01-19 | 2022-05-03 | 江西广源化工有限责任公司 | Composite inorganic flame retardant and preparation method thereof |
| CN114790394A (en) * | 2021-07-07 | 2022-07-26 | 合肥中科阻燃新材料有限公司 | Composite environment-friendly flame retardant for A-grade fireproof composite board and preparation method thereof |
-
2019
- 2019-12-23 CN CN201911340885.9A patent/CN111073055A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266536A (en) * | 2020-11-05 | 2021-01-26 | 广东天雄新材料科技股份有限公司 | Carrier-free weather-resistant PP flame-retardant master batch and preparation method and application thereof |
| CN112724465A (en) * | 2020-12-29 | 2021-04-30 | 宁波艾克姆新材料有限公司 | Flame-retardant silane crosslinked nano modified polyolefin pre-dispersed master batch auxiliary |
| CN114790394A (en) * | 2021-07-07 | 2022-07-26 | 合肥中科阻燃新材料有限公司 | Composite environment-friendly flame retardant for A-grade fireproof composite board and preparation method thereof |
| CN114426702A (en) * | 2022-01-19 | 2022-05-03 | 江西广源化工有限责任公司 | Composite inorganic flame retardant and preparation method thereof |
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Application publication date: 20200428 |