CN110591210A - Preparation method of environment-friendly flame-retardant material - Google Patents
Preparation method of environment-friendly flame-retardant material Download PDFInfo
- Publication number
- CN110591210A CN110591210A CN201810598839.8A CN201810598839A CN110591210A CN 110591210 A CN110591210 A CN 110591210A CN 201810598839 A CN201810598839 A CN 201810598839A CN 110591210 A CN110591210 A CN 110591210A
- Authority
- CN
- China
- Prior art keywords
- flame retardant
- pentaerythritol
- environment
- master batch
- density polyethylene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 65
- 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 56
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- WLTAYLKDPLWQMU-UHFFFAOYSA-N N1=C(N)N=C(N)N=C1N.B(O)(O)OCC(CO)(CO)CO Chemical compound N1=C(N)N=C(N)N=C1N.B(O)(O)OCC(CO)(CO)CO WLTAYLKDPLWQMU-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229920000092 linear low density polyethylene Polymers 0.000 claims abstract description 25
- 239000004707 linear low-density polyethylene Substances 0.000 claims abstract description 25
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004327 boric acid Substances 0.000 claims abstract description 13
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 26
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 24
- XRILDTYZSWVEPL-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propoxy]boronic acid Chemical compound OCC(CO)(CO)COB(O)O XRILDTYZSWVEPL-UHFFFAOYSA-N 0.000 claims description 11
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001746 injection moulding Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000008096 xylene Substances 0.000 claims description 8
- 229920003023 plastic Polymers 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- -1 pentaerythritol borate ester Chemical class 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 abstract description 14
- 239000001301 oxygen Substances 0.000 abstract description 14
- 239000007789 gas Substances 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052796 boron Inorganic materials 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910052736 halogen Inorganic materials 0.000 description 8
- 150000002367 halogens Chemical class 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000012796 inorganic flame retardant Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 150000001638 boron Chemical class 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/56—Preparation of melamine
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/04—Esters of boric acids
-
- 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
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- 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
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
-
- 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
- C08K5/55—Boron-containing compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention belongs to the technical field of flame retardant materials, and particularly relates to a preparation method of an environment-friendly flame retardant material. The invention takes pentaerythritol, boric acid and melamine as raw materials to synthesize a boron intumescent flame retardant which integrates a carbon source, an acid source and a gas source, namely pentaerythritol borate melamine salt, and then pentaerythritol borate melamine salt is taken as a flame retardant to be added into linear low density polyethylene to prepare the linear low density polyethylene with flame retardant property, wherein the linear low density polyethylene has excellent flame retardant property and the oxygen index of 28%.
Description
Technical Field
The invention belongs to the technical field of flame retardant materials, and particularly relates to a preparation method of an environment-friendly flame retardant material.
Background
With the improvement of national economic level and the development of scientific technology, high polymer materials represented by plastic products, rubber products and fiber products are widely applied in daily life and play an increasingly important role in the life of people. The application range of the high polymer materials in daily life of people is wider and wider, and great convenience is brought, however, most of the high polymer materials mainly comprise carbon and hydrogen elements, and because the high polymer materials have the characteristic of extremely easy combustion, the combustion speed is very high, and great fire hazard safety hazards are hidden, meanwhile, the high polymer materials generate a great amount of toxic and harmful smoke and gas in the combustion process, great damage is caused to the natural ecological environment where people depend on to live while great risks are hidden for the life health of people, and great attention is paid to the flame retardant industry of the high polymer materials all over the world.
Flame retardants can be divided into two main categories according to product properties: organic type flame retardants and inorganic type flame retardants. The organic flame retardant mainly comprises a halogen-containing organic compound, a nitrogen-containing organic compound and a phosphorus-containing organic compound, generally, the organic flame retardant has good compatibility in a high polymer material, the halogen flame retardant represented by organic bromide and organic chloride accounts for about 51 percent of the organic flame retardant, the phosphorus flame retardant represented by organic phosphate and organic phosphorus-nitrogen compound accounts for about 22 percent of the organic flame retardant, the nitrogen flame retardant represented by cyanuric acid and melamine compound accounts for about 20 percent of the organic flame retardant, and the other type flame retardant represented by organic phosphorus/nitrogen intumescent compound accounts for about 7 percent of the organic flame retardant. The inorganic flame retardant mainly uses inorganic metals such as antimony oxide, aluminum hydroxide, magnesium hydroxide, red phosphorus, boron compounds and the like or inorganic non-metals as raw materials, and the inorganic flame retardant is generally compounded with other types of flame retardants in the use process due to poor compatibility with high polymer materials.
At present, a halogen flame retardant occupies a large amount in an organic flame retardant system in China, although the halogen flame retardant generates a large amount of corrosive toxic and harmful gas through decomposition reaction under the condition of heating, and simultaneously generates dense smoke, the life health of people is seriously affected, and the natural environment is also seriously polluted, the halogen flame retardant has the advantages of good compatibility, strong stability, wide application range, high cost performance and the like, so that the halogen flame retardant becomes the most common organic flame retardant in the application range so far. Since 1990, the European Union underwent hazard evaluation of some halogen flame retardants with the widest application range and halogen/phosphorus composite flame retardants, for example, evaluation of decabromodiphenyl oxide for 10 years, and underwent more than 1100 detection experiments, and the conclusion was that organic bromine flame retardants have hazard or carcinogenicity to human bodies, and the evaluation results are successively published.
Therefore, the development of halogen-free flame retardant with low price, no toxicity and no pollution is urgent, and the development trend of the flame retardant industry in future is the high-efficiency halogen-free environment-friendly flame retardant regardless of the environmental protection or the progress of the flame retardant technology.
Disclosure of Invention
The invention aims to provide an environment-friendly halogen-free flame retardant preparation method.
The invention takes pentaerythritol, boric acid and melamine as raw materials to synthesize a boron intumescent flame retardant which integrates a carbon source, an acid source and a gas source, namely pentaerythritol borate melamine salt, and then pentaerythritol borate melamine salt is taken as a flame retardant to be added into linear low density polyethylene to prepare the linear low density polyethylene with flame retardant property, and the flame retardant property is excellent.
The invention realizes the aim through the following technical scheme, and the preparation method of the environment-friendly flame retardant material comprises the following steps:
1) adding boric acid, pentaerythritol and xylene into a reactor for high-temperature reaction, and decompressing and steaming out the xylene after the reaction is finished to obtain pentaerythritol borate;
2) dispersing pentaerythritol borate into n-heptane, uniformly stirring and dispersing, adding melamine, stirring for 20-30min, and then decompressing and distilling off the n-heptane to obtain a pentaerythritol borate melamine salt precursor;
3) curing the pentaerythritol borate melamine salt precursor in an oven at a high temperature for 2-3h to obtain pentaerythritol borate melamine salt;
4) respectively extruding and granulating pentaerythritol borate melamine salt and linear low-density polyethylene by adopting a double-screw extruder to obtain pentaerythritol borate melamine salt master batch and linear low-density polyethylene master batch; the pentaerythritol borate melamine salt master batch and the linear low-density polyethylene master batch are subjected to melt blending and then are subjected to injection molding by a plastic injection molding machine to obtain the environment-friendly flame retardant material.
Preferably, the molar ratio of the boric acid to the pentaerythritol in the step 1) is 1:1, the high-temperature reaction temperature is 100-115 ℃.
Preferably, the weight ratio of the pentaerythritol borate to the melamine in the step 2) is pentaerythritol borate: melamine =2: 1; the curing temperature of the high-temperature curing is 140 ℃.
Preferably, the pentaerythritol borate melamine salt master batch in the environment-friendly flame retardant material in the step 3) is 12-15% of the weight of the linear low density polyethylene master batch, and more preferably 13%.
The technical advantages of the invention are as follows:
the invention synthesizes boron series intumescent flame retardant pentaerythritol borate melamine salt which integrates a carbon source, an acid source and a gas source by taking pentaerythritol, boric acid and melamine as raw materials, and then adds the pentaerythritol borate melamine salt as a flame retardant into linear low density polyethylene to prepare the linear low density polyethylene with flame retardant property, wherein the linear low density polyethylene has excellent flame retardant property and the oxygen index of 28%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
Example 1
1) Adding 10g of boric acid into a reactor, dispersing the boric acid into 100mL of xylene, then adding pentaerythritol (with the same molar weight as the boric acid) to react at the high temperature of 110 ℃ for 2h, and decompressing and distilling off the xylene after the reaction is finished to obtain pentaerythritol borate;
2) dispersing 10g of pentaerythritol borate into 100mL of n-heptane, uniformly stirring and dispersing, adding 5g of melamine, stirring for 20-30min, and then decompressing and distilling off the n-heptane to obtain a pentaerythritol borate melamine salt precursor; curing the pentaerythritol borate melamine salt precursor in an oven at 140 ℃ for 2-3h to obtain pentaerythritol borate melamine salt;
3) respectively extruding and granulating pentaerythritol borate melamine salt and linear low-density polyethylene by adopting a double-screw extruder to obtain pentaerythritol borate melamine salt master batch and linear low-density polyethylene master batch; the pentaerythritol borate melamine salt master batch and the linear low-density polyethylene master batch are subjected to melt blending and then are subjected to injection molding by a plastic injection molding machine to obtain the environment-friendly flame retardant material (the pentaerythritol borate melamine salt master batch accounts for 13% of the weight of the linear low-density polyethylene master batch).
Example 2
1) Adding 10g of boric acid into a reactor, dispersing the boric acid in 100ml of xylene, then adding pentaerythritol (with the same molar weight as the boric acid) to react at the high temperature of 110 ℃ for 2 hours, and decompressing and distilling off the xylene after the reaction is finished to obtain pentaerythritol borate;
2) dispersing 10g of pentaerythritol borate into 100ml of n-heptane, uniformly stirring and dispersing, adding 5g of melamine, stirring for 20-30min, and then decompressing and distilling off the n-heptane to obtain a pentaerythritol borate melamine salt precursor; curing the pentaerythritol borate melamine salt precursor in an oven at 140 ℃ for 2-3h to obtain pentaerythritol borate melamine salt;
3) respectively extruding and granulating pentaerythritol borate melamine salt and linear low-density polyethylene by adopting a double-screw extruder to obtain pentaerythritol borate melamine salt master batch and linear low-density polyethylene master batch; the pentaerythritol borate melamine salt master batch and the linear low-density polyethylene master batch are subjected to melt blending, and then the environment-friendly flame retardant material is obtained through injection molding by a plastic injection molding machine (the pentaerythritol borate melamine salt master batch accounts for 15% of the weight of the linear low-density polyethylene master batch).
The flame retardant property of the environment-friendly flame retardant material prepared in example 1 was measured by an oxygen number method:
the Oxygen Index (OI) refers to the lowest oxygen concentration required for the flamed combustion of a polymeric material in a stream of oxygen and nitrogen mixture under specified conditions. The oxygen index is determined according to GB/T2406.1-2008 (determination of the combustion behaviour of plastics by the oxygen index method) and is expressed as the percentage by volume of oxygen. A higher oxygen index indicates that the polymeric material is less flammable, and a lower oxygen index indicates that the polymeric material is more flammable. The oxygen-nitrogen mixture in the transparent combustion cylinder flows upward in a laminar flow manner, and then the jig is installed in the combustion cylinder, and the measurement is performed at room temperature after the standard sample is fixed. The top surface of the standard bar was lit, the flame contacted the top surface of the bar for a maximum of 30 seconds and removed every 5 seconds to see if the standard bar burned. This ensures that the sample temperature is not too high and a lower OI value is obtained. The calculation formula is as follows:
OI=O2/（O2+N2）×100%
wherein OI is the oxygen index, O2Is the volume occupied by oxygen in the oxygen-nitrogen mixed gas flow, N2Is the volume occupied by nitrogen in the oxygen-nitrogen mixture gas flow.
The oxygen index test result of the environment-friendly flame-retardant material is 28%, and the environment-friendly flame-retardant material belongs to a flame-retardant high polymer material.
Although the embodiments of the present invention have been described in detail, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of an environment-friendly flame retardant material is characterized by comprising the following steps: the method comprises the following steps:
1) adding boric acid, pentaerythritol and xylene into a reactor for high-temperature reaction, and decompressing and steaming out the xylene after the reaction is finished to obtain pentaerythritol borate;
2) dispersing pentaerythritol borate into n-heptane, uniformly stirring and dispersing, adding melamine, stirring for 20-30min, and then decompressing and distilling off the n-heptane to obtain a pentaerythritol borate melamine salt precursor;
3) curing the pentaerythritol borate melamine salt precursor in an oven at a high temperature for 2-3h to obtain pentaerythritol borate melamine salt;
4) respectively extruding and granulating pentaerythritol borate melamine salt and linear low-density polyethylene by adopting a double-screw extruder to obtain pentaerythritol borate melamine salt master batch and linear low-density polyethylene master batch; the pentaerythritol borate melamine salt master batch and the linear low-density polyethylene master batch are subjected to melt blending and then are subjected to injection molding by a plastic injection molding machine to obtain the environment-friendly flame retardant material.
2. The method for preparing the environment-friendly flame retardant material according to claim 1, characterized in that: in the step 1), the molar ratio of the boric acid to the pentaerythritol is 1:1, and the high-temperature reaction temperature is 100-115 ℃.
3. The method for preparing the environment-friendly flame retardant material according to claim 1, characterized in that: in the step 2), the weight ratio of the pentaerythritol borate to the melamine is as follows: pentaerythritol borate ester: melamine =2: 1; the curing temperature of the high-temperature curing is 140 ℃.
4. The method for preparing the environment-friendly flame retardant material according to claim 1, characterized in that: in the step 3), in the environment-friendly flame retardant material, the pentaerythritol borate melamine salt master batch accounts for 12-15% of the weight of the linear low-density polyethylene master batch.
5. The method for preparing the environment-friendly flame retardant material according to claim 4, characterized in that: in the step 3), the pentaerythritol borate melamine salt master batch in the environment-friendly flame retardant material accounts for 13% of the weight of the linear low-density polyethylene master batch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810598839.8A CN110591210A (en) | 2018-06-12 | 2018-06-12 | Preparation method of environment-friendly flame-retardant material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810598839.8A CN110591210A (en) | 2018-06-12 | 2018-06-12 | Preparation method of environment-friendly flame-retardant material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110591210A true CN110591210A (en) | 2019-12-20 |
Family
ID=68848647
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810598839.8A Withdrawn CN110591210A (en) | 2018-06-12 | 2018-06-12 | Preparation method of environment-friendly flame-retardant material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110591210A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111423463A (en) * | 2020-05-26 | 2020-07-17 | 南通纺织丝绸产业技术研究院 | Preparation method and application of reactive boron-containing flame retardant |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928420A (en) * | 2009-06-24 | 2010-12-29 | 上海金发科技发展有限公司 | Halogen-free flame-retardant expanded polyethylene composition and preparation method thereof |
| CN102964376A (en) * | 2012-11-29 | 2013-03-13 | 石家庄启宏橡塑制品有限公司 | Preparation method and application of halogen-free environment-friendly flame retardant |
| JP5179731B2 (en) * | 2005-08-11 | 2013-04-10 | ポリプラスチックス株式会社 | Flame retardant resin composition |
| CN103339172A (en) * | 2011-01-31 | 2013-10-02 | 巴斯夫欧洲公司 | Methods of flame retarding polyethylene processed at high temperatures |
| CN105037911A (en) * | 2015-07-28 | 2015-11-11 | 浙江万马高分子材料有限公司 | Easy-peel highlighted silane crosslinking flame-retardant polyolefin insulation material, preparation method and application thereof |
-
2018
- 2018-06-12 CN CN201810598839.8A patent/CN110591210A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5179731B2 (en) * | 2005-08-11 | 2013-04-10 | ポリプラスチックス株式会社 | Flame retardant resin composition |
| CN101928420A (en) * | 2009-06-24 | 2010-12-29 | 上海金发科技发展有限公司 | Halogen-free flame-retardant expanded polyethylene composition and preparation method thereof |
| CN103339172A (en) * | 2011-01-31 | 2013-10-02 | 巴斯夫欧洲公司 | Methods of flame retarding polyethylene processed at high temperatures |
| CN102964376A (en) * | 2012-11-29 | 2013-03-13 | 石家庄启宏橡塑制品有限公司 | Preparation method and application of halogen-free environment-friendly flame retardant |
| CN105037911A (en) * | 2015-07-28 | 2015-11-11 | 浙江万马高分子材料有限公司 | Easy-peel highlighted silane crosslinking flame-retardant polyolefin insulation material, preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘玉涛: "一种硼系环保无卤阻燃剂的合成与应用", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 张亚通，等: "硼系膨胀型阻燃剂的合成与性能", 《塑料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111423463A (en) * | 2020-05-26 | 2020-07-17 | 南通纺织丝绸产业技术研究院 | Preparation method and application of reactive boron-containing flame retardant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102875982A (en) | In-situ modified halogen-free flame retardant thermoplastic resin composition and preparation method thereof | |
| CN103073788B (en) | Weather-resistant moisture-resistant halogen-free flame-retardant polypropylene mixture and preparation method thereof | |
| CN102219957B (en) | Functional masterbatch of halogen-free intumescent flame retardant, and preparation method thereof | |
| CN101343392B (en) | Halogen-free flame-proof reinforced polypropylene composite material and preparation thereof | |
| CN113930044B (en) | Flame-retardant ABS composite material, preparation method and application thereof | |
| CN113248912B (en) | Flame-retardant nylon material for battery pack shell and preparation method thereof | |
| CN113956291A (en) | Diacid monomer, copolymerization flame retardant nylon prepared from diacid monomer and copolymerization flame retardant nylon and method | |
| CN110734596A (en) | halogen-free flame-retardant low-density polyethylene material, and preparation method and application thereof | |
| CN115260754A (en) | High-toughness halogen-free flame-retardant PA66 material and preparation method thereof | |
| CN101624457B (en) | Environmental protection based red mud combination modification synergism fire-retardant polyethylene | |
| CN114479286A (en) | Low-smoke halogen-free flame-retardant polypropylene composition and preparation method and application thereof | |
| CN103740038A (en) | High-glossiness halogen-free flame-retardant ABS material and preparation method thereof | |
| CN107629450A (en) | A kind of environment friendly non-halogen type fiber glass reinforced polyamide fire retardant | |
| CN110591210A (en) | Preparation method of environment-friendly flame-retardant material | |
| CN113801162A (en) | Diacid monomer, copolymerization flame retardant nylon and preparation method thereof | |
| CN103467852B (en) | A kind of Polypropylene flame-retardant plastic | |
| CN109575324B (en) | Chemically modified transparent flame-retardant PET master batch and manufacturing method and application thereof | |
| CN110591154A (en) | Environment-friendly flame-retardant material | |
| CN113956294B (en) | Special flame retardant for polyoxymethylene and preparation method thereof | |
| CN108570205A (en) | A kind of Flameproof styrenic composition and preparation method thereof | |
| CN105111728A (en) | Preparation process for flame-retardant nylon resin | |
| CN114196200B (en) | Preparation method of flame retardant-free low-flammability polyamide material | |
| CN101608049A (en) | A kind of halogen-free flame-retardant ABS resin and preparation method thereof | |
| CN111234367A (en) | Flame-retardant antistatic polypropylene film composite material and preparation method thereof | |
| CN115505172A (en) | Halogen-free flame retardant and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20191220 |