CN113881445A - Preparation method of magnesium-based flame-retardant material - Google Patents
Preparation method of magnesium-based flame-retardant material Download PDFInfo
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- CN113881445A CN113881445A CN202111152606.3A CN202111152606A CN113881445A CN 113881445 A CN113881445 A CN 113881445A CN 202111152606 A CN202111152606 A CN 202111152606A CN 113881445 A CN113881445 A CN 113881445A
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- flame retardant
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- 239000011777 magnesium Substances 0.000 title claims abstract description 62
- 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 52
- 239000003063 flame retardant Substances 0.000 title claims abstract description 52
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 69
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000008367 deionised water Substances 0.000 claims abstract description 34
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 34
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 20
- 238000005485 electric heating Methods 0.000 claims abstract description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- AXLHVTKGDPVANO-UHFFFAOYSA-N methyl 2-amino-3-[(2-methylpropan-2-yl)oxycarbonylamino]propanoate Chemical compound COC(=O)C(N)CNC(=O)OC(C)(C)C AXLHVTKGDPVANO-UHFFFAOYSA-N 0.000 claims abstract description 13
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000012467 final product Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 14
- 239000000084 colloidal system Substances 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000004945 emulsification Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 8
- 239000000779 smoke Substances 0.000 abstract description 8
- 238000002485 combustion reaction Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000979 retarding effect Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention discloses a preparation method of a magnesium-based flame retardant material, which comprises the following raw materials in parts by weight: 100-200 parts of sodium hydroxide, 50-100 parts of magnesium chloride, 25-50 parts of superfine activated carbon, a plurality of parts of deionized water, 2.5-5 parts of sodium stearate, 2.5-5 parts of silane coupling agent and 2.5-5 parts of magnesium oleate; in the preparation process of the magnesium-based flame-retardant material, the digital display constant-temperature electric heating jacket is firstly heated to 150 ℃, then the mixture of sodium hydroxide, magnesium chloride and deionized water as raw materials is heated under the condition of keeping the temperature unchanged, and an electric stirrer is used for stirring, so that the product Mg (OH) caused by uneven temperature is avoided2The particle size of the superfine activated carbon is different, the quality of a final product is influenced, the superfine activated carbon is added into the product, the product and the superfine activated carbon are uniformly mixed through a mixer to obtain the final product, and the added superfine activated carbon adsorbs and purifies smoke smell generated by combustion in the flame-retardant processAnd perfect the flame retardant effect.
Description
Technical Field
The invention relates to the field of preparation of flame retardant materials, in particular to a preparation method of a magnesium-based flame retardant material.
Background
The magnesium-based flame retardant mainly plays a role in flame retarding a material through a condensed phase flame retarding mechanism, and mainly adopts Mg (OH)2Decompose to absorb heat and generate water to achieve flame retardant effect, and Mg (OH)2As a flame retardant, the flame retardant does not generate toxic gas in the flame retardant process, is green and environment-friendly, has various preparation schemes, and mainly adopts NaOH and MgCI in the scheme2Preparing raw materials by a hydrothermal synthesis method, and modifying the surface of a prepared product to obtain a final product;
firstly, in the production process of the existing magnesium-based flame retardant material, the digital display constant temperature electric heating sleeve heats the mixture of sodium hydroxide, magnesium chloride and deionized water at the temperature rising stage to obtain Mg (OH)2Colloidal particle size non-uniform, Mg (OH) obtained before constant temperature2The colloid has too large particle size, is not suitable to be used as a flame retardant, affects the quality of products, and the existing magnesium-based flame retardant material has a smoke suppression effect but cannot adsorb and purify smoke smell and the like generated by combustion.
Disclosure of Invention
The invention aims to provide a preparation method of a magnesium-based flame retardant material, which solves the problem that in the production process of the existing magnesium-based flame retardant material, a digital display constant temperature electric heating sleeve heats a mixture of sodium hydroxide, magnesium chloride and deionized water at a temperature rising stage, so that the obtained Mg (OH)2Colloidal particle size non-uniform, Mg (OH) obtained before constant temperature2The colloid has too large particle size, is not suitable to be used as a flame retardant, and affects the quality of products, and the prior magnesium-based flame retardant material has the smoke suppression effect but cannot adsorb and purify smoke smell and the like generated by combustion; compared with the traditional preparation method of the magnesium-based flame retardant material, in the preparation process of the magnesium-based flame retardant material, the digital display constant temperature electric heating jacket is firstly heated to 150 ℃, and then the temperature is maintained to be unchanged for sodium hydroxide and chlorine serving as raw materialsHeating the mixture of magnesium oxide and deionized water, and stirring with an electric stirrer to avoid Mg (OH) product caused by uneven temperature2The particle size of the superfine activated carbon is different, the quality of a final product is influenced, the superfine activated carbon is added into the product, the product and the superfine activated carbon are uniformly mixed through a mixer, the final product is obtained, and in the flame retardant process, smoke smell generated by combustion is adsorbed and purified through the added superfine activated carbon, so that the flame retardant effect is improved.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the magnesium-based flame retardant material comprises the following raw materials in parts by weight: 100 portions of sodium hydroxide, 50 portions to 100 portions of magnesium chloride, 25 portions to 50 portions of superfine active carbon, a plurality of portions of deionized water, 2.5 portions to 5 portions of sodium stearate, 2.5 portions to 5 portions of silane coupling agent and 2.5 portions to 5 portions of magnesium oleate, and the preparation method specifically comprises the following steps:
the method comprises the following steps: adding sodium hydroxide and magnesium chloride into a round-bottom flask, adding 150 parts of deionized water into the round-bottom flask, and shaking the round-bottom flask to mix the sodium hydroxide, the magnesium chloride and the deionized water;
step two: starting a digital display constant temperature electric heating jacket, continuously heating to 150 ℃, keeping the temperature unchanged, then placing a round-bottom flask on the digital display constant temperature electric heating jacket, inserting an electric stirrer into the round-bottom flask, starting the electric stirrer, and heating a mixture of sodium hydroxide, magnesium chloride and deionized water in the round-bottom flask at the temperature of 150 ℃ in a stirring state, wherein the reaction formula is MgCl2+2NaOH＝Mg(OH)2+2NaCl；
Step three: cooling the reaction product in the second step, adding deionized water for washing, washing away sodium chloride in the reactant, and filtering the reactant to obtain Mg (OH)2A colloid;
step four: the resulting Mg (OH)2Drying the colloid in a drying oven, and drying to obtain Mg (OH)2Pouring the mixture, sodium stearate, a silane coupling agent and magnesium oleate into an emulsifying machine for emulsification treatment;
step five: pouring out the emulsified product in the step, washing with deionized water, and then drying to obtain a final product, namely the magnesium-based flame retardant;
step six: and D, pouring the magnesium-based flame retardant obtained in the fifth step and the superfine activated carbon into a mixer for mixing to obtain the magnesium-based flame retardant material.
Further, the magnesium-based flame retardant material comprises the following components in parts by weight: 100 parts of sodium hydroxide, 50 parts of magnesium chloride, 25 parts of superfine activated carbon, a plurality of parts of deionized water, 2.5 parts of sodium stearate, 2.5 parts of a silane coupling agent and 2.5 parts of magnesium oleate;
further, the time for maintaining the constant-temperature electric heating jacket at 150 ℃ and the stirring time of the electric stirrer in the step two are both 1.5h, and the rotating speed of the electric stirrer is 2000 r/min.
Further, the temperature of the reactant after cooling in the third step is not higher than 40 ℃, the washing standard is deionized water washing, the filtrate is kept stand for 3min, the supernatant is not turbid, and the washing frequency is not lower than 3 times.
Further, the step four contains Mg (OH)2The drying temperature of the colloid is 200 ℃, the drying time is 1h, Mg (OH)2And the mixing and emulsifying time of the sodium stearate, the silane coupling agent and the magnesium oleate is 3 h.
Further, the washing standard in the fifth step is that after the filtrate is washed by deionized water, the supernatant is not turbid after the filtrate is kept stand for 2min, the washing frequency is not lower than 5 times, the drying temperature is 100 ℃, and the drying time is 1.5 h.
The invention has the beneficial effects that:
1. compared with the traditional preparation method of the magnesium-based flame retardant material, in the preparation process of the magnesium-based flame retardant material, the digital display constant temperature electric heating jacket is firstly heated to 150 ℃, then the mixture of sodium hydroxide, magnesium chloride and deionized water as raw materials is heated under the condition of keeping the temperature unchanged, and an electric stirrer is used for stirring, so that the product Mg (OH) caused by uneven temperature is avoided2The particle size of the product is different, so that the quality of the final product is influenced;
2. superfine activated carbon is added into the product, and the product and the superfine activated carbon are uniformly mixed through a mixer to obtain a final product, and during the flame-retardant process, the added superfine activated carbon adsorbs and purifies smoke smell generated by combustion, so that the flame-retardant effect is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the magnesium-based flame retardant material comprises the following raw materials in parts by weight: 100 portions of sodium hydroxide, 50 portions to 100 portions of magnesium chloride, 25 portions to 50 portions of superfine active carbon, a plurality of portions of deionized water, 2.5 portions to 5 portions of sodium stearate, 2.5 portions to 5 portions of silane coupling agent and 2.5 portions to 5 portions of magnesium oleate, and the preparation method specifically comprises the following steps:
the method comprises the following steps: adding sodium hydroxide and magnesium chloride into a round-bottom flask, adding 150 parts of deionized water into the round-bottom flask, and shaking the round-bottom flask to mix the sodium hydroxide, the magnesium chloride and the deionized water;
step two: starting a digital display constant temperature electric heating jacket, continuously heating to 150 ℃, keeping the temperature unchanged, then placing a round-bottom flask on the digital display constant temperature electric heating jacket, inserting an electric stirrer into the round-bottom flask, starting the electric stirrer, and heating a mixture of sodium hydroxide, magnesium chloride and deionized water in the round-bottom flask at the temperature of 150 ℃ in a stirring state, wherein the reaction formula is MgCl2+2NaOH＝Mg(OH)2+2NaCl；
Step three: cooling the reaction product in the second step, adding deionized water for washing, washing away sodium chloride in the reactant, and filtering the reactant to obtain Mg (OH)2A colloid;
step four: the resulting Mg (OH)2Drying the colloid in a drying oven, and drying to obtain Mg (OH)2Pouring the mixture, sodium stearate, a silane coupling agent and magnesium oleate into an emulsifying machine for emulsification treatment;
step five: pouring out the emulsified product in the step, washing with deionized water, and then drying to obtain a final product, namely the magnesium-based flame retardant;
step six: and D, pouring the magnesium-based flame retardant obtained in the fifth step and the superfine activated carbon into a mixer for mixing to obtain the magnesium-based flame retardant material.
The magnesium-based flame-retardant material comprises the following components in parts by weight: 100 parts of sodium hydroxide, 50 parts of magnesium chloride, 25 parts of superfine activated carbon, a plurality of parts of deionized water, 2.5 parts of sodium stearate, 2.5 parts of a silane coupling agent and 2.5 parts of magnesium oleate;
in the second step, the time for maintaining the constant temperature electric heating jacket at 150 ℃ and the stirring time of the electric stirrer are both 1.5h, and the rotating speed of the electric stirrer is 2000 r/min.
In the third step, the temperature of the cooled reactant is not higher than 40 ℃, the washing standard is deionized water washing, the upper layer liquid is not turbid after the filtrate is kept stand for 3min, and the washing frequency is not lower than 3 times.
Step four Mg (OH)2The drying temperature of the colloid is 200 ℃, the drying time is 1h, Mg (OH)2And the mixing and emulsifying time of the sodium stearate, the silane coupling agent and the magnesium oleate is 3 h.
And the washing standard in the step five is that after deionized water washing, the filtrate is kept stand for 2min, the supernatant is not turbid, the washing frequency is not lower than 5 times, the drying temperature is 100 ℃, and the drying time is 1.5 h.
Compared with the traditional preparation method of the magnesium-based flame retardant material, in the preparation process of the magnesium-based flame retardant material, the digital display constant temperature electric heating jacket is firstly heated to 150 ℃, then the mixture of sodium hydroxide, magnesium chloride and deionized water as raw materials is heated under the condition of keeping the temperature unchanged, and an electric stirrer is used for stirring, so that the product Mg (OH) caused by uneven temperature is avoided2The particle size of the product is different, so that the quality of the final product is influenced; adding superfine active carbon into the product, uniformly mixing the product and the superfine active carbon by a mixer to obtain a final product, and in the process of flame retardance, combusting the produced superfine active carbonThe smoke smell is adsorbed and purified, and the flame retardant effect is improved.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. A method for preparing a magnesium-based flame retardant material is characterized by comprising the following steps: the magnesium-based flame-retardant material is composed of the following raw materials in parts by weight: 100 portions of sodium hydroxide, 50 portions to 100 portions of magnesium chloride, 25 portions to 50 portions of superfine active carbon, a plurality of portions of deionized water, 2.5 portions to 5 portions of sodium stearate, 2.5 portions to 5 portions of silane coupling agent and 2.5 portions to 5 portions of magnesium oleate, and the preparation method specifically comprises the following steps:
the method comprises the following steps: adding sodium hydroxide and magnesium chloride into a round-bottom flask, adding 150 parts of deionized water into the round-bottom flask, and shaking the round-bottom flask to mix the sodium hydroxide, the magnesium chloride and the deionized water;
step two: starting a digital display constant temperature electric heating jacket, continuously heating to 150 ℃, keeping the temperature unchanged, then placing a round-bottom flask on the digital display constant temperature electric heating jacket, inserting an electric stirrer into the round-bottom flask, starting the electric stirrer, and heating a mixture of sodium hydroxide, magnesium chloride and deionized water in the round-bottom flask at the temperature of 150 ℃ in a stirring state, wherein the reaction formula is MgCl2+2NaOH＝Mg(OH)2+2NaCl；
Step three: cooling the reaction product in the second step, adding deionized water for washing, washing away sodium chloride in the reactant, and filtering the reactant to obtain Mg (OH)2A colloid;
step four: the resulting Mg (OH)2Drying the colloid in a drying oven, and drying to obtain Mg (OH)2Pouring the mixture, sodium stearate, a silane coupling agent and magnesium oleate into an emulsifying machine for emulsification treatment;
step five: pouring out the emulsified product in the step, washing with deionized water, and then drying to obtain a final product, namely the magnesium-based flame retardant;
step six: and D, pouring the magnesium-based flame retardant obtained in the fifth step and the superfine activated carbon into a mixer for mixing to obtain the magnesium-based flame retardant material.
2. The method for preparing the magnesium-based flame retardant material according to claim 1, wherein the magnesium-based flame retardant material comprises the following components in parts by weight: 100 parts of sodium hydroxide, 50 parts of magnesium chloride, 25 parts of superfine activated carbon, a plurality of parts of deionized water, 2.5 parts of sodium stearate, 2.5 parts of silane coupling agent and 2.5 parts of magnesium oleate.
3. The method for preparing a magnesium-based flame retardant material as claimed in claim 1, wherein: in the second step, the time for maintaining the digital display constant-temperature electric heating jacket at 150 ℃ and the stirring time of the electric stirrer are both 1.5h, and the rotating speed of the electric stirrer is 2000 r/min.
4. The method for preparing a magnesium-based flame retardant material as claimed in claim 1, wherein: and in the third step, the temperature of the cooled reactants is not higher than 40 ℃, the washing standard is that after deionized water is used for washing, the filtrate is kept stand for 3min, the supernatant is not turbid, and the washing frequency is not lower than 3 times.
5. The method for preparing a magnesium-based flame retardant material as claimed in claim 1, wherein: mg (OH) in the fourth step2The drying temperature of the colloid is 200 ℃, the drying time is 1h, Mg (OH)2And the mixing and emulsifying time of the sodium stearate, the silane coupling agent and the magnesium oleate is 3 h.
6. The method for preparing a magnesium-based flame retardant material as claimed in claim 1, wherein: and the washing standard in the step five is that after deionized water is washed, the filtrate is kept stand for 2min, the supernatant is not turbid, the washing frequency is not lower than 5 times, the drying temperature is 100 ℃, and the drying time is 1.5 h.
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Application publication date: 20220104 |