CN116948261A - Magnesium hydroxide/organic silicon composite flame retardant capable of improving flame retardant efficiency - Google Patents
Magnesium hydroxide/organic silicon composite flame retardant capable of improving flame retardant efficiency Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 144
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 140
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 108
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 108
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 108
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 21
- 229910052710 silicon Inorganic materials 0.000 title claims description 21
- 239000010703 silicon Substances 0.000 title claims description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000002156 mixing Methods 0.000 claims abstract description 57
- 229910000077 silane Inorganic materials 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000000975 co-precipitation Methods 0.000 claims abstract description 9
- 238000003980 solgel method Methods 0.000 claims abstract description 9
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- 150000001343 alkyl silanes Chemical class 0.000 claims abstract description 5
- 238000009827 uniform distribution Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 37
- 238000000227 grinding Methods 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 28
- 239000003381 stabilizer Substances 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 239000004014 plasticizer Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 17
- 229910052731 fluorine Inorganic materials 0.000 claims description 14
- 239000011737 fluorine Substances 0.000 claims description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 7
- 230000000704 physical effect Effects 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 239000001488 sodium phosphate Substances 0.000 claims description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 7
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 7
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 7
- 229920001971 elastomer Polymers 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000005060 rubber Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000005696 Diammonium phosphate Substances 0.000 claims description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 5
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 5
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 229920002635 polyurethane Polymers 0.000 claims description 5
- 239000004814 polyurethane Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000004566 building material Substances 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 125000001153 fluoro group Chemical group F* 0.000 claims description 3
- 238000001879 gelation Methods 0.000 claims description 3
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000004753 textile Substances 0.000 claims description 3
- 238000000518 rheometry Methods 0.000 claims description 2
- 230000002708 enhancing effect Effects 0.000 claims 1
- 125000004185 ester group Chemical group 0.000 claims 1
- 239000004593 Epoxy Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012796 inorganic flame retardant Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- -1 epoxysilanes Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
Classifications
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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
- C08K9/06—Ingredients treated with organic substances with silicon-containing 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
-
- 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
- C08K3/32—Phosphorus-containing 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
-
- 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
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/324—Alkali metal phosphate
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention relates to the technical field of composite flame retardants, in particular to a magnesium hydroxide/organosilicon composite flame retardant for improving flame retardant efficiency, which comprises magnesium hydroxide and organosilicon, wherein the content of the magnesium hydroxide is between 40 and 70 percent, the content of the organosilicon is between 20 and 50 percent, the organosilicon is silane, the specific type of the silane comprises aminosilane, epoxy silane, alkylsilane or arylsilane, the silane can effectively improve the thermal stability and mechanical property of the flame retardant, and in actual operation, the silane can be mixed with the magnesium hydroxide by a solution mixing method, a solution dipping method, a sol-gel method and a coprecipitation method for ensuring the uniform distribution of the silane in the flame retardant. The composite flame retardant has excellent heat stability and weather resistance, and can be suitable for fireproof materials in high temperature, humidity and other severe environments.
Description
Technical Field
The invention relates to the technical field of composite flame retardants, in particular to a magnesium hydroxide/organic silicon composite flame retardant capable of improving flame retardant efficiency.
Background
The conventional flame retardant mainly comprises two types of inorganic and organic, inorganic flame retardants such as hydrated alumina, magnesium hydroxide and the like, and organic flame retardants such as halides, phosphate esters and the like, wherein magnesium hydroxide is widely used in various fireproof materials due to the advantages of no toxicity, no public hazard, no smoke and the like.
However, the conventional flame retardant has problems in that, for example, the flame retardant effect of the inorganic flame retardant is generally poor, a large addition amount is required, which affects the mechanical properties and processability of the material, and the organic flame retardant, although having a good flame retardant effect, may generate toxic smoke during high temperature combustion, which poses a threat to the environment and human health.
In order to solve the above problems, a method using a magnesium hydroxide/organosilicon composite flame retardant has been proposed, which combines the advantages of magnesium hydroxide and organosilicon, has both good flame retardant effect and reduced smoke generation, and simultaneously, has excellent thermal stability and weather resistance due to the combination of silane and magnesium hydroxide, thereby greatly improving the application range and effect of the flame retardant.
However, the existing preparation method of the magnesium hydroxide/organic silicon composite flame retardant is still to be improved, and the existing preparation method generally comprises the steps of grinding, mixing, heat treatment and the like, and a large amount of energy sources are consumed in the steps, and the preparation process is complex and low in efficiency, so that how to improve the preparation efficiency and the flame retardant effect of the magnesium hydroxide/organic silicon composite flame retardant is an important research subject at present.
Disclosure of Invention
Based on the above objects, the present invention provides a magnesium hydroxide/silicone composite flame retardant with improved flame retardant efficiency.
The magnesium hydroxide/organic silicon composite flame retardant with high flame retarding efficiency includes magnesium hydroxide in 40-70 wt% and organic silicon in 20-50 wt%.
Further, the organic silicon is silane, specific types of silane include aminosilane, epoxy silane, alkylsilane or arylsilane, the silane will effectively improve the thermal stability and mechanical properties of the flame retardant, in practice, the silane will be mixed with magnesium hydroxide by means of solution mixing, solution impregnation, sol-gel method, co-precipitation method for ensuring uniform distribution in the flame retardant, wherein:
mixing the solution: firstly, respectively dissolving magnesium hydroxide and silane in a proper solvent, then mixing the two solutions together for reaction to ensure that the silane and the magnesium hydroxide are fully reacted and uniformly distributed, and after the reaction is finished, obtaining the magnesium hydroxide flame retardant containing the silane through steps of separation, washing, drying and the like;
solution impregnation: firstly, putting magnesium hydroxide particles into a solution containing silane, then soaking the magnesium hydroxide particles at normal temperature to enable the silane to soak and adhere to the surfaces of the magnesium hydroxide particles, and taking out the particles and drying the particles after soaking is finished to obtain the magnesium hydroxide flame retardant containing the silane;
sol-gel process: firstly, dissolving silane in a solvent, then adding magnesium hydroxide particles, mixing and reacting at normal temperature to form magnesium hydroxide sol containing silane, and then obtaining the magnesium hydroxide flame retardant containing silane through the steps of gelation, drying, heat treatment and the like;
coprecipitation method: firstly, magnesium hydroxide particles and silane are added into a precipitant solution at the same time, then the reaction is carried out at normal temperature, the silane and the magnesium hydroxide are precipitated together, and after the precipitation is finished, the magnesium hydroxide flame retardant containing the silane is obtained through the steps of separation, washing, drying and the like.
Further, the magnesium hydroxide is nano magnesium hydroxide with a particle size of 50-150 nanometers, the nano magnesium hydroxide can enhance the thermal stability and flame retardant property of the flame retardant, the surface area of the nano magnesium hydroxide is increased in the range, chemical bonds are formed with the organosilicon, and the particle size of the nano magnesium hydroxide also affects the physical properties of the flame retardant, wherein the physical properties include rheological property and filling property.
Further, the composite flame retardant also comprises a stabilizer, the dosage of the stabilizer is between 1 and 5 percent, the stabilizer is used for improving the thermal stability of the flame retardant, and the stabilizer is a phosphate stabilizer, and specifically comprises trisodium phosphate or diammonium phosphate.
Furthermore, the composite flame retardant also comprises a plasticizer, the dosage of the plasticizer is between 2 and 8 percent, the plasticizer is an ester plasticizer, in particular to phthalate or phosphate, the plasticizer is used for improving the rheological property of the flame retardant, and the plasticity and toughness of the flame retardant can be improved, so that the flame retardant is easier to flow in the processing process, and the processing and forming of materials such as plastics, rubber and the like are facilitated.
Further, the composite flame retardant also comprises a weather-proof agent, the dosage of the weather-proof agent is between 1 and 5 percent, wherein the weather-proof agent is fluorine-containing weather-proof agent, and particularly comprises fluorine-containing polyester or fluorine-containing polyurethane, and the weather-proof agent is used for preventing environmental factors such as ultraviolet rays, humidity, high temperature and the like from damaging the flame retardant, so that the service life and flame retardant effect of the flame retardant are improved.
Further, the preparation method of the composite flame retardant comprises the following steps:
firstly, mixing and stirring 60% of magnesium hydroxide and 30% of aminosilane, wherein a solution dipping method is adopted during mixing, high-speed stirring and mixing are adopted, the stirring speed is set at 800rpm, and the mixing time is set at 60 minutes;
then adding 5% of stabilizer, wherein the stabilizer is trisodium phosphate, and stirring and mixing until uniform;
then, 3% of a plasticizer, which is phthalate, was added, and then mixed for 40 minutes.
Then adding 2% of weather-proof agent which is fluorine polyester, and finally mixing for 30 minutes.
And finally, grinding and drying the mixture, wherein a high-speed grinding machine is selected as grinding equipment, the grinding time is set to be 2 hours, the grinding speed is set to be 2000rpm, the drying step adopts vacuum drying, the drying temperature is set to be 120 ℃, and the drying time is set to be 6 hours, so that the magnesium hydroxide/organic silicon composite flame retardant is obtained.
Further, the flame retardant is applied to plastics, rubber, textiles and building material fireproof materials.
The invention has the following beneficial effects:
the invention combines the advantages of inorganic and organic flame retardants, has good flame retardant property, can reduce the generation of toxic smog, and particularly, has excellent heat stability and weather resistance because of the combination of silane and magnesium hydroxide, and can be suitable for fireproof materials in high temperature, humidity and other severe environments.
According to the invention, the performance of the flame retardant can be regulated and controlled by selecting and adjusting the proportion of the magnesium hydroxide and the organic silicon and adding the stabilizer, the plasticizer and the weather-resistant agent, so that the requirements of different application occasions are met, for example, the flame retardant performance of the flame retardant can be improved by increasing the content of the magnesium hydroxide; by adjusting the type and content of the organosilicon, the thermal stability and weather resistance of the flame retardant can be improved; by adding stabilizers, plasticizers and weathering agents, the mechanical properties, rheology and durability of the flame retardant can be further improved, which makes the application of the flame retardant more extensive and flexible.
The invention can reduce the preparation cost and is also beneficial to improving the production efficiency, in the preparation process, the flame retardant with uniform and fine particles can be obtained by optimizing parameters of steps such as mixing, grinding, drying and the like, which is beneficial to improving the dispersibility and flame retardant effect of the flame retardant in the fireproof material, and in addition, the performance and application performance of the flame retardant can be further optimized by changing the preparation method, such as adopting a solution mixing method, a solution dipping method, a sol-gel method, a coprecipitation method and the like.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a preparation method of a composite flame retardant according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the mixing method according to an embodiment of the present invention.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
As shown in fig. 1-2, a magnesium hydroxide/organosilicon composite flame retardant for improving flame retardant efficiency comprises magnesium hydroxide and organosilicon, wherein the content of the magnesium hydroxide is between 40% and 70%, and the content of the organosilicon is between 20% and 50%.
The organosilicon is a silane, the specific types of which include aminosilanes, epoxysilanes, alkylsilanes or arylsilanes, which will effectively improve the thermal stability and mechanical properties of the flame retardant, wherein the choice and amount of silane will depend on the application requirements and process conditions of the final flame retardant, and in practice the silane will be mixed with magnesium hydroxide by means of solution mixing, solution impregnation, sol-gel process, co-precipitation process for ensuring a homogeneous distribution thereof in the flame retardant, wherein:
mixing the solution: firstly, respectively dissolving magnesium hydroxide and silane in a proper solvent, then mixing the two solutions together for reaction to ensure that the silane and the magnesium hydroxide are fully reacted and uniformly distributed, and after the reaction is finished, obtaining the magnesium hydroxide flame retardant containing the silane through steps of separation, washing, drying and the like;
solution impregnation: firstly, putting magnesium hydroxide particles into a solution containing silane, then soaking the magnesium hydroxide particles at normal temperature to enable the silane to soak and adhere to the surfaces of the magnesium hydroxide particles, and taking out the particles and drying the particles after soaking is finished to obtain the magnesium hydroxide flame retardant containing the silane;
sol-gel process: firstly, dissolving silane in a solvent, then adding magnesium hydroxide particles, mixing and reacting at normal temperature to form magnesium hydroxide sol containing silane, and then obtaining the magnesium hydroxide flame retardant containing silane through the steps of gelation, drying, heat treatment and the like;
coprecipitation method: firstly, magnesium hydroxide particles and silane are added into a precipitant solution at the same time, then the reaction is carried out at normal temperature, the silane and the magnesium hydroxide are precipitated together, and after the precipitation is finished, the magnesium hydroxide flame retardant containing the silane is obtained through the steps of separation, washing, drying and the like.
The above methods can achieve effective mixing of silane and magnesium hydroxide to improve the flame retardant and physical properties of the composite flame retardant, however, each method has applicable conditions and limitations, and the appropriate method should be selected according to actual requirements and conditions.
The magnesium hydroxide is nano magnesium hydroxide with a particle size of 50-150 nanometers, the nano magnesium hydroxide can enhance the thermal stability and flame retardant property of the flame retardant, the surface area of the nano magnesium hydroxide in the range is increased, chemical bonds are formed with organic silicon, the thermal stability of the flame retardant is further improved, the particle size of the nano magnesium hydroxide also affects the physical properties of the flame retardant, wherein the physical properties comprise rheological property and filling property, and therefore, the control of the particle size is also very important.
The composite flame retardant also comprises a stabilizer, the dosage of the stabilizer is between 1 and 5 percent, the stabilizer is used for improving the thermal stability of the flame retardant, the stabilizer is a phosphate stabilizer, and specifically comprises trisodium phosphate or diammonium phosphate, and the stabilizer can improve the thermal stability of the flame retardant, so that the flame retardant is stable in a high-temperature environment and is not easy to thermally degrade, thereby improving the flame retardant effect of the flame retardant.
The composite flame retardant also comprises a plasticizer, the dosage of the plasticizer is between 2 and 8 percent, the plasticizer is an ester plasticizer, and is specifically phthalate or phosphate, the plasticizer is used for improving the rheological property of the flame retardant, and can also improve the plasticity and toughness of the flame retardant, so that the flame retardant is easier to flow in the processing process, and is convenient for the processing and forming of materials such as plastics, rubber and the like.
The composite flame retardant also comprises a weather-proof agent, the consumption of the weather-proof agent is between 1 and 5 percent, the weather-proof agent is fluorine-containing weather-proof agent, the weather-proof agent specifically comprises fluorine-containing polyester or fluorine-containing polyurethane, and the weather-proof agent is used for preventing environmental factors such as ultraviolet rays, humidity, high temperature and the like from damaging the flame retardant, so that the service life and the flame retardant effect of the flame retardant are improved, and the stability of the flame retardant in a severe environment is improved.
The flame retardant is applied to fireproof materials of plastics, rubber, textiles and building materials, and has the advantages of wide application in various fireproof materials due to the flame retardant efficiency, thermal stability, weather resistance and compatibility with various base materials, and excellent performance can be obtained according to different base materials and flame retardant requirements by changing the composition and the proportion of the flame retardant.
Example 1:
in this example, a magnesium hydroxide/organosilicon composite flame retardant was prepared, comprising the following specific steps:
firstly, mixing and stirring 60% of magnesium hydroxide and 30% of aminosilane, wherein a solution dipping method is adopted during mixing, high-speed stirring and mixing are adopted, the stirring speed is set at 800rpm, and the mixing time is set at 60 minutes;
then adding 5% of stabilizer, wherein the stabilizer is trisodium phosphate, and stirring and mixing until uniform;
then adding 3% of plasticizer which is phthalate, and mixing for 40 minutes;
adding 2% of weather-proof agent which is fluorine polyester, and finally mixing for 30 minutes;
and finally, grinding and drying the mixture, wherein a high-speed grinding machine is selected as grinding equipment, the grinding time is set to be 2 hours, the grinding speed is set to be 2000rpm, the drying step adopts vacuum drying, the drying temperature is set to be 120 ℃, and the drying time is set to be 6 hours, so that the magnesium hydroxide/organic silicon composite flame retardant is obtained.
Example 2:
in this example, a magnesium hydroxide/organosilicon composite flame retardant was prepared, comprising the following specific steps:
firstly, 50% of nano magnesium hydroxide and 40% of epoxy silane are measured, a solution dipping method is adopted during mixing, high-speed stirring and mixing are adopted, the stirring speed is set at 800rpm, and the mixing time is set at 60 minutes;
then adding 5% of stabilizer, wherein the stabilizer is diammonium phosphate, and stirring and mixing until the mixture is uniform;
then adding 4% of plasticizer which is phthalate, and mixing for 40 minutes;
then adding 1% of weather-proof agent which is fluoropolyester, and mixing for 30 minutes;
and finally, grinding and drying the mixture, wherein a high-speed grinding machine is selected as grinding equipment, the grinding time is set to be 2 hours, the grinding speed is set to be 2000rpm, the drying step adopts vacuum drying, the drying temperature is set to be 120 ℃, and the drying time is set to be 6 hours, so that the magnesium hydroxide/organic silicon composite flame retardant is obtained.
Example 3:
in this example, a magnesium hydroxide/organosilicon composite flame retardant was prepared, comprising the following specific steps:
firstly, measuring 70% of nano magnesium hydroxide and 20% of alkylsilane, mixing by adopting a sol-gel method, stirring and mixing at a high speed, wherein the stirring speed is set at 800rpm, and the mixing time is set at 60 minutes;
then adding 4% of stabilizer, wherein the stabilizer is trisodium phosphate, and stirring and mixing until uniform;
then adding 5% of plasticizer which is phosphate, and mixing for 40 minutes;
then adding 1% of weather-proof agent which is fluorine-containing polyurethane, and mixing for 30 minutes;
and finally, grinding and drying the mixture, wherein a high-speed grinding machine is selected as grinding equipment, the grinding time is set to be 2 hours, the grinding speed is set to be 2000rpm, the drying step is vacuum drying, the drying temperature is set to be 120 ℃, and the drying time is set to be 6 hours, so that the magnesium hydroxide/organic silicon composite flame retardant is obtained.
Example 4:
in this example, a magnesium hydroxide/organosilicon composite flame retardant was prepared, comprising the following specific steps:
mixing and stirring 60% of magnesium hydroxide and 30% of epoxy silane, adopting a coprecipitation method during mixing, adopting high-speed stirring and mixing, setting the stirring speed at 800rpm, and setting the mixing time at 60 minutes;
then adding 5% of diammonium phosphate, stirring and mixing until the mixture is uniform;
then adding 3% of phosphate plasticizer, and mixing for 40 minutes;
then adding 2% of fluorine-containing polyurethane weather-proof agent, and finally mixing for 30 minutes;
and finally, grinding and drying the mixture, wherein a high-speed grinding machine is selected as grinding equipment, the grinding time is set to be 2 hours, the grinding speed is set to be 2000rpm, the drying step adopts vacuum drying, the drying temperature is set to be 120 ℃, and the drying time is set to be 6 hours, so that the magnesium hydroxide/organic silicon composite flame retardant is obtained.
The following table is the experimental data table
This table now shows the flame retardant efficiency and thermal stability of each example, with higher percentages indicating better flame retardant efficiency and thermal stability indicating the highest temperature that the flame retardant can withstand without significant performance loss.
From this table we can see that example 1 has the highest flame retardant efficiency and thermal stability, so we can consider example 1 as the best example because the proportions of magnesium hydroxide and silicone, as well as the types and amounts of stabilizer, plasticizer, weatherproofing agent in example 1, all reach the best balance, thus optimizing the properties of the flame retardant produced.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (8)
1. The magnesium hydroxide/organic silicon composite flame retardant is characterized by comprising magnesium hydroxide and organic silicon, wherein the content of the magnesium hydroxide is between 40 and 70 percent, and the content of the organic silicon is between 20 and 50 percent.
2. A magnesium hydroxide/silicone composite flame retardant having improved flame retardant efficiency according to claim 1, wherein said silicone is a silane of the specific type comprising aminosilane, epoxysilane, alkylsilane or arylsilane which will be effective to improve the thermal stability and mechanical properties of the flame retardant, in practice the silane will be mixed with magnesium hydroxide by solution mixing, solution impregnation, sol-gel process, co-precipitation process for ensuring uniform distribution thereof in the flame retardant, wherein:
mixing the solution: firstly, respectively dissolving magnesium hydroxide and silane in a proper solvent, then mixing the two solutions together for reaction to ensure that the silane and the magnesium hydroxide are fully reacted and uniformly distributed, and after the reaction is finished, obtaining the magnesium hydroxide flame retardant containing the silane through steps of separation, washing, drying and the like;
solution impregnation: firstly, putting magnesium hydroxide particles into a solution containing silane, then soaking the magnesium hydroxide particles at normal temperature to enable the silane to soak and adhere to the surfaces of the magnesium hydroxide particles, and taking out the particles and drying the particles after soaking is finished to obtain the magnesium hydroxide flame retardant containing the silane;
sol-gel process: firstly, dissolving silane in a solvent, then adding magnesium hydroxide particles, mixing and reacting at normal temperature to form magnesium hydroxide sol containing silane, and then obtaining the magnesium hydroxide flame retardant containing silane through the steps of gelation, drying, heat treatment and the like;
coprecipitation method: firstly, magnesium hydroxide particles and silane are added into a precipitant solution at the same time, then the reaction is carried out at normal temperature, the silane and the magnesium hydroxide are precipitated together, and after the precipitation is finished, the magnesium hydroxide flame retardant containing the silane is obtained through the steps of separation, washing, drying and the like.
3. A magnesium hydroxide/silicone composite flame retardant having improved flame retardant efficiency according to claim 1, wherein the magnesium hydroxide is nano magnesium hydroxide having a particle size between 50 and 150 nanometers, wherein the nano magnesium hydroxide is capable of enhancing the thermal stability and flame retardant properties of the flame retardant, wherein the nano magnesium hydroxide has an increased surface area that forms chemical bonds with the silicone, and wherein the particle size of the nano magnesium hydroxide is also capable of affecting the physical properties of the flame retardant, wherein the physical properties include rheology and fillability.
4. The magnesium hydroxide/organosilicon composite flame retardant for improving flame retardant efficiency according to claim 1, further comprising a stabilizer, wherein the stabilizer is used for improving thermal stability of the flame retardant, and the stabilizer is phosphate stabilizer, specifically trisodium phosphate or diammonium phosphate.
5. The magnesium hydroxide/organic silicon composite flame retardant for improving flame retardant efficiency according to claim 1, further comprising a plasticizer, wherein the amount of the plasticizer is between 2% and 8%, the plasticizer is an ester plasticizer, specifically phthalate or phosphate, the plasticizer is used for improving rheological property of the flame retardant, and the plasticity and toughness of the flame retardant can be improved, so that the flame retardant is easier to flow in a processing process, and is convenient for processing and forming of materials such as plastics, rubber and the like.
6. The magnesium hydroxide/organic silicon composite flame retardant for improving flame retardant efficiency according to claim 1, further comprising a weather-proof agent, wherein the weather-proof agent is fluorine-containing weather-proof agent, and specifically comprises fluorine-containing polyester or fluorine-containing polyurethane, and the weather-proof agent is used for preventing environmental factors such as ultraviolet rays, humidity and high temperature from damaging the flame retardant, so that the service life and flame retardant effect of the flame retardant are improved.
7. The magnesium hydroxide/organosilicon composite flame retardant for improving flame retardant efficiency according to claim 1, wherein the preparation method of the composite flame retardant comprises the following steps:
firstly, mixing and stirring 60% of magnesium hydroxide and 30% of aminosilane, wherein a solution dipping method is adopted during mixing, high-speed stirring and mixing are adopted, the stirring speed is set at 800rpm, and the mixing time is set at 60 minutes;
then adding 5% of stabilizer, wherein the stabilizer is trisodium phosphate, and stirring and mixing until uniform;
then adding 3% of plasticizer which is phthalate, and mixing for 40 minutes;
adding 2% of weather-proof agent which is fluorine polyester, and finally mixing for 30 minutes;
and finally, grinding and drying the mixture, wherein a high-speed grinding machine is selected as grinding equipment, the grinding time is set to be 2 hours, the grinding speed is set to be 2000rpm, the drying step adopts vacuum drying, the drying temperature is set to be 120 ℃, and the drying time is set to be 6 hours, so that the magnesium hydroxide/organic silicon composite flame retardant is obtained.
8. The magnesium hydroxide/silicone composite flame retardant with improved flame retardant efficiency according to claim 1, wherein the flame retardant is used in materials for plastics, rubber, textiles and building materials for fire protection.
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