CN118292297A - Washable flame retardant applied to filter material and application method thereof - Google Patents
Washable flame retardant applied to filter material and application method thereof Download PDFInfo
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- CN118292297A CN118292297A CN202410438678.1A CN202410438678A CN118292297A CN 118292297 A CN118292297 A CN 118292297A CN 202410438678 A CN202410438678 A CN 202410438678A CN 118292297 A CN118292297 A CN 118292297A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 74
- 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 72
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000178 monomer Substances 0.000 claims abstract description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000758 substrate Substances 0.000 claims abstract description 34
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 26
- 239000010703 silicon Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- QHGULWZMFCZMSR-UHFFFAOYSA-N dichlorophosphorylperoxybenzene Chemical compound ClP(Cl)(=O)OOC1=CC=CC=C1 QHGULWZMFCZMSR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 14
- 239000004593 Epoxy Substances 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 10
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 10
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- WGYFACNYUJGZQO-UHFFFAOYSA-N aminomethanetriol Chemical compound NC(O)(O)O WGYFACNYUJGZQO-UHFFFAOYSA-N 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 238000007142 ring opening reaction Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000001276 controlling effect Effects 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- HFWWEMPLBCKNNM-UHFFFAOYSA-N n-[bis(hydroxyamino)methyl]hydroxylamine Chemical compound ONC(NO)NO HFWWEMPLBCKNNM-UHFFFAOYSA-N 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000835 fiber Substances 0.000 abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- -1 siloxane structures Chemical group 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000002390 rotary evaporation Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Filtering Materials (AREA)
Abstract
The invention relates to a washable flame retardant applied to a filter material and an application method thereof, belonging to the technical field of flame retardants. The flame retardant comprises the following raw materials in percentage by weight: 55-70% of hydrophilic flame retardant, 5-10% of ethanol, 0.1-0.5% of hydrochloric acid and the balance of water; the hydrophilic flame retardant is obtained by heating and reacting hydrophilic silicon monomer and phenoxy dichlorophosphate under the action of aluminum chloride and nitrogen protection. The self-made hydrophilic flame retardant has good hydrophilicity, and the dispersion process of the self-made hydrophilic flame retardant does not involve harmful organic solvents; secondly, in the curing process, through silanol bonds hydrolyzed by siloxane structures in molecules of the modified phenolic resin, the modified phenolic resin is easily grafted with hydroxyl groups on the fiber surface of the filter substrate, so that the modified phenolic resin is cured on the surface of the filter substrate, the waterproof function of the modified phenolic resin is realized, and the problems in the background art are solved.
Description
Technical Field
The invention belongs to the technical field of flame retardants, and particularly relates to a washable flame retardant applied to a filter material and an application method thereof.
Background
In the existing product, the air filter paper for the engine needs to meet the foreign DIN53438-3 test standard, and the filter material for the filter element still has the function of not attenuating the flame retardant performance after soaking in water for 24 hours. At present, the imported filter material mainly comprises wood pulp filter base material, phenolic resin and solvent type flame retardant, and has the problem of environmental pollution caused by volatilization of harmful solvent and formaldehyde. Therefore, there is a need for a flame retardant that is resistant to water washing after curing and that is environmentally friendly for filter material applications.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a washable flame retardant applied to a filter material and an application method thereof.
The invention provides a washable flame retardant for filtering material application, which comprises the following raw materials in percentage by weight: 55-70% of hydrophilic flame retardant, 5-10% of cosolvent, 0.1-1% of hydrochloric acid and the balance of water;
the hydrophilic flame retardant is obtained by heating reaction of hydrophilic silicon monomer and phenoxy dichlorophosphate under the action of aluminum chloride and nitrogen protection;
the hydrophilic silicon monomer is shown below;
Wherein R is OCH 3 or OCH 2CH3.
Further, the reaction of the hydrophilic silicon monomer and the phenoxy dichlorophosphate comprises:
dropwise adding phenoxy dichlorophosphate into a mixed system of hydrophilic silicon monomer and aluminum chloride at 60-65 ℃ under the protection of nitrogen, wherein a tail gas recovery device is arranged on the mixed system, reacting for 4-6 hours under the heat preservation, heating to 200 ℃, continuously stirring and reacting for 3-5 hours to obtain a reactant, dissolving the reactant with chloroform, precipitating with methanol, filtering and drying to obtain a hydrophilic flame retardant; in the reaction, hydroxyl in the hydrophilic silicon monomer and chloro in phenoxy dichlorophosphate are utilized to react, so that the hydrophilic silicon monomer is connected with a phosphate structure, the obtained hydrophilic flame retardant has the characteristic of a phosphorus flame retardant, meanwhile, the molecular structure of the hydrophilic flame retardant contains carboxyl and an active structure of siloxane, the carboxyl imparts hydrophilicity, the active structure of the siloxane imparts grafting performance with the fiber surface of the filter substrate, and the washing resistance is imparted.
Further, the molar ratio of the hydrophilic silicon monomer to the phenoxy dichlorophosphate to the aluminum chloride is 1-1.5:1:0.01-0.02.
Further, the hydrophilic silicon monomer is generated by a ring-opening reaction between a hydrophilic monomer generated by the reaction of phthalic anhydride and trihydroxy aminomethane and an epoxy silane coupling agent, and in the ring-opening reaction, the ring-opening reaction between the hydroxyl of the hydrophilic silicon monomer and the epoxy group of the epoxy silane coupling agent is utilized, so that the hydrophilic monomer is connected with a siloxane structure, and the active structure of the hydrophilic silicon monomer siloxane is endowed.
Further, the reaction of the hydrophilic monomer and the epoxy silane coupling agent includes:
Mixing hydrophilic monomer and ethanol, regulating pH of the mixed system to 9-11, controlling reaction temperature to 50-60 ℃, dripping epoxy silane coupling agent, continuously stirring for reaction for 4-6h after dripping, stopping reaction, regulating solution to neutrality with hydrochloric acid, adding acetone for precipitation separation, dissolving and washing the precipitate product with ethanol, precipitating and separating with acetone again, and vacuum drying to obtain hydrophilic silicon monomer.
Further, the molar ratio of the hydrophilic monomer to the epoxy silane coupling agent is 1:1.
Further, the reaction of phthalic anhydride and trihydroxy aminomethane comprises:
Uniformly mixing phthalic anhydride, trihydroxy aminomethane and ethanol, heating and refluxing for reaction for 8-24h, stopping the reaction, recovering ethanol by rotary evaporation, and drying to obtain the hydrophilic monomer.
Further, the molar ratio of phthalic anhydride to trihydroxy aminomethane is 1:1.
The molecular structure of the hydrophilic monomer is shown as follows;
Further, the concentration of the hydrochloric acid is 0.1-1mol/L.
Further, the solvent is an alcoholic solvent, such as ethanol, ethylene glycol, glycerol, preferably ethanol.
A second object of the present invention is to provide a method for the application of a water-wash resistant flame retardant for filter material applications, comprising: immersing the filter substrate into the raw material mixed solution with the following weight percentages: 55-70% of hydrophilic flame retardant, 5-10% of cosolvent, 0.1-1% of hydrochloric acid and the balance of water; and preserving the temperature at 50-70 ℃ for 30-90min, taking out, drying, baking, washing and drying to obtain the flame-retardant filter substrate.
The invention has the beneficial effects that:
According to the washable flame retardant applied to the filter material, the self-made hydrophilic flame retardant has good hydrophilicity, can be well dispersed in a mixed system of water and alcohol solvents, and does not involve harmful organic solvents in the dispersion process; secondly, in the curing process, through silanol bonds hydrolyzed by siloxane structures in molecules of the epoxy resin, the epoxy resin is easily grafted with hydroxyl groups on the fiber surface of the filter substrate, so that the epoxy resin is cured on the surface of the filter substrate, and the water-resistant function of the epoxy resin is realized, and phenolic resin is not required to be cured, so that formaldehyde is not volatilized, and the problems in the background art are solved;
The self-made hydrophilic flame retardant is characterized in that in the process of being applied to a filter substrate, under an acidic condition, a siloxane structure in a branched chain form is subjected to grafting curing reaction with hydroxyl groups on the surface of the filter substrate fiber, and self-hyperbranched reaction (dehydration hyperbranched reaction between silanol bonds) is also carried out, so that hydrophilic flame retardant molecules are bridged (dehydration condensation of silanol bonds formed by siloxane hydrolysis in one hydrophilic flame retardant molecule and silanol bonds formed by siloxane hydrolysis in the other hydrophilic flame retardant molecule) to promote the hydrophilic flame retardant molecules to form an interpenetrating network on the surface of the fiber, and then the interpenetrating flame retardant layer is formed by curing on the surface of the filter substrate, and the interpenetrating flame retardant layer contains a repeating unit consisting of hydrophilic silicon monomers and phenoxy dichlorophosphate, can simultaneously play the characteristics of a silicon flame retardant and a phosphorus flame retardant, and has excellent flame retardant performance.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of hydrophilic flame retardant:
The first step: uniformly mixing 1mol of phthalic anhydride, 1mol of trihydroxy aminomethane and 300mL of ethanol, heating and refluxing for reaction for 8 hours, stopping the reaction, recovering the ethanol by rotary evaporation, and drying to obtain a hydrophilic monomer;
And a second step of: mixing the hydrophilic monomer obtained in the first step with 350mL of ethanol, regulating the pH of a mixed system to 10, controlling the reaction temperature to 50 ℃, dropwise adding 1mol of epoxy silane coupling agent (KH-560), continuously stirring for reaction for 6 hours after the dropwise adding is completed, stopping the reaction, regulating the solution to be neutral by using hydrochloric acid, adding acetone for precipitation and separation, dissolving and washing a precipitation product by using ethanol, precipitating and separating by using acetone again, and vacuum drying to obtain a hydrophilic silicon monomer;
And a third step of: and (3) dropwise adding 1mol of phenoxy dichlorophosphate into a mixed system of the hydrophilic silicon monomer obtained in the second step and 1.45g of aluminum chloride under the protection of nitrogen and at 60 ℃ and with a tail gas recovery device, reacting at the temperature of the mixed system for 6 hours, heating to 200 ℃, continuing to stir for 3 hours until no bubbles are generated (hydrogen chloride), obtaining a reactant, dissolving the reactant with chloroform, precipitating with methanol, filtering and drying to obtain the hydrophilic flame retardant.
Example 2
Preparation of hydrophilic flame retardant:
Preparation of hydrophilic flame retardant:
the first step: uniformly mixing 1mol of phthalic anhydride, 1mol of trihydroxy aminomethane and 300mL of ethanol, heating and refluxing for reaction for 24 hours, stopping the reaction, recovering the ethanol by rotary evaporation, and drying to obtain a hydrophilic monomer;
And a second step of: mixing the hydrophilic monomer obtained in the first step with 350mL of ethanol, regulating the pH of a mixed system to 10.5, controlling the reaction temperature to 60 ℃, dropwise adding 1mol of epoxy silane coupling agent (gamma-glycidol ether oxypropyl triethoxysilane), continuously stirring for reaction for 4 hours after the dropwise adding is completed, stopping the reaction, regulating the solution to be neutral by hydrochloric acid, adding acetone for precipitation and separation, dissolving and washing a precipitate product by ethanol, precipitating and separating by acetone again, and vacuum drying to obtain the hydrophilic silicon monomer;
And a third step of: and (3) dropwise adding 1mol of phenoxy dichlorophosphate into a mixed system of the hydrophilic silicon monomer obtained in the second step and 1.45g of aluminum chloride under the protection of nitrogen and at the temperature of 65 ℃ and with a tail gas recovery device, reacting at the temperature of 4 hours while keeping the temperature, continuously stirring and reacting for 5 hours until no bubbles are generated (hydrogen chloride), obtaining a reactant, dissolving the reactant with chloroform, precipitating with methanol, filtering and drying to obtain the hydrophilic flame retardant.
Comparative example 1
The hydrophilic silicon monomer prepared in the second step of example 1 was used as a hydrophilic flame retardant.
The filter substrates used in the following examples and comparative examples were wood pulp filter substrates.
Example 3
Taking: the raw materials by weight percentage are as follows: 55% of the hydrophilic flame retardant prepared in example 1, 5% of ethanol, 0.1% of hydrochloric acid and the balance of water;
And (3) treating a filter substrate: immersing the filtering substrate in the mixed solution of the hydrophilic flame retardant, ethanol, hydrochloric acid and water which are taken out of the filtering substrate; and preserving heat at 50 ℃ for 90min, taking out, drying (110 ℃ for 120 s), baking (165 ℃ for 150 s), washing and drying (60 ℃) to obtain the flame-retardant filter substrate.
Example 4
Taking: the raw materials by weight percentage are as follows: 60% of the hydrophilic flame retardant prepared in example 2, 8% of ethanol, 0.4% of hydrochloric acid and the balance of water;
And (3) treating a filter substrate: immersing the filtering substrate in the mixed solution of the hydrophilic flame retardant, ethanol, hydrochloric acid and water which are taken out of the filtering substrate; and preserving heat at 60 ℃ for 60min, taking out, drying (110 ℃ for 120 s), baking (165 ℃ for 150 s), washing and drying (60 ℃) to obtain the flame-retardant filter substrate.
Example 5
Taking: the raw materials by weight percentage are as follows: 70% of the hydrophilic flame retardant prepared in the example 1, 10% of ethanol, 1% of hydrochloric acid and the balance of water;
and (3) treating a filter substrate: immersing the filtering substrate in the mixed solution of the hydrophilic flame retardant, ethanol, hydrochloric acid and water which are taken out of the filtering substrate; and preserving the heat at 70 ℃ for 30min, taking out, drying (110 ℃ for 120 s), baking (165 ℃ for 150 s), washing and drying (60 ℃) to obtain the flame-retardant filter substrate.
Comparative example 2
Taking: the hydrophilic flame retardant in example 3 was replaced with the hydrophilic flame retardant in comparative example 1, and the rest was the same as the raw material in example 3;
And (3) treating a filter substrate: the same filter substrate treatment as in example 3 was performed.
Comparative example 3
Taking: the same as in example 3;
And (3) treating a filter substrate: immersing the filter substrate in the mixture of the hydrophilic flame retardant, ethanol, hydrochloric acid and water, keeping the room temperature for 90min, taking out, drying (110 ℃ for 120 s), baking (165 ℃ for 150 s), washing and drying (60 ℃) to obtain the flame-retardant filter substrate.
Comparative example 4
Taking: the same as in comparative example 2;
and (3) treating a filter substrate: the same filter substrate treatment as in comparative example 3.
Performance test obtained for the filter materials obtained in examples 3 to 5 and comparative examples 2 to 4:
Combustion performance test: the limiting oxygen index (LOI%) is used for evaluation, and is measured according to the requirements in the GB/T5454 textile combustion performance measurement-oxygen index method;
The method for washing the flame-retardant fabric comprises the following steps: washing is carried out according to the requirements of a household washing process before the GB/T17595 fabric burning test.
The results of the above performance tests are shown in Table 1.
TABLE 1
As can be seen from the data in table 1, the filter substrates obtained in examples 3 to 5 of the present invention have excellent flame retardant properties, and the resulting flame retardant properties are wash resistant.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (10)
1. The washable flame retardant for the filter material is characterized by comprising the following raw materials in percentage by weight: 55-70% of hydrophilic flame retardant, 5-10% of cosolvent, 0.1-0.5% of hydrochloric acid and the balance of water;
the hydrophilic flame retardant is obtained by heating reaction of hydrophilic silicon monomer and phenoxy dichlorophosphate under the action of aluminum chloride and nitrogen protection;
The molecular structural formula of the hydrophilic silicon monomer is shown as follows:
Wherein R is OCH 3 or OCH 2CH3.
2. The washable flame retardant for filter materials of claim 1, wherein the molar ratio of hydrophilic silicon monomer, phenoxy dichlorophosphate, aluminum chloride is 1-1.5:1:0.01-0.02.
3. A water wash resistant flame retardant for use in filter materials according to claim 1, wherein said reaction of hydrophilic silicon monomer and phenoxy dichlorophosphate comprises:
And (3) dropwise adding phenoxy dichlorophosphate into a mixed system of hydrophilic silicon monomers and aluminum chloride under the protection of nitrogen at 60-65 ℃, reacting for 4-6h under the heat preservation, heating to 200 ℃, continuously stirring and reacting for 3-5h to obtain a reactant, dissolving the reactant with chloroform, precipitating with methanol, filtering and drying to obtain the hydrophilic flame retardant.
4. The washable flame retardant for filter materials of claim 1, wherein the hydrophilic silicon monomer is formed by a ring-opening reaction of a hydrophilic monomer formed by the reaction of phthalic anhydride and tris-hydroxy-aminomethane with an epoxy silane coupling agent.
5. A water wash resistant flame retardant for filtration material applications according to claim 4, wherein the ring opening reaction of the hydrophilic monomer and the epoxy silane coupling agent comprises:
Mixing hydrophilic monomer and ethanol, regulating pH of the mixed system to 9-11, controlling reaction temperature to 50-60 ℃, dripping epoxy silane coupling agent, continuously stirring for reaction for 4-6h after dripping, stopping reaction, and performing post-treatment to obtain hydrophilic silicon monomer.
6. A washable flame retardant for use in filter materials according to claim 4, wherein the molar ratio of hydrophilic monomer to epoxy silane coupling agent in the ring opening reaction of the hydrophilic monomer and epoxy silane coupling agent is 1:1.
7. A water wash resistant flame retardant for use in filter materials according to claim 4, wherein said reaction of phthalic anhydride and tris-hydroxy-aminomethane comprises:
uniformly mixing phthalic anhydride, trihydroxy aminomethane and ethanol, heating and refluxing for 8-24h, stopping the reaction, and drying to obtain the hydrophilic monomer.
8. A water wash resistant flame retardant for use in a filter material according to claim 7, wherein the molar ratio of phthalic anhydride to trihydroxyaminomethane is 1:1.
9. The washable flame retardant for use in filter materials according to claim 1, wherein the concentration of hydrochloric acid is 0.1-1mol/L and the dissolution promoter is ethanol.
10. The method of using a water-washable flame retardant for filter materials of claim 1, comprising: immersing the filter substrate in a mixed solution of a hydrophilic flame retardant, a cosolvent, hydrochloric acid and water, preserving the temperature at 50-70 ℃ for 30-90min, taking out, drying, baking, washing and drying to obtain the flame-retardant filter substrate.
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| KR20120060980A (en) * | 2010-10-01 | 2012-06-12 | 유한회사 피피지코리아 | Copolymer of organic silane and phosphorous ester and the process of producing a flame retardant clear paint |
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| US20190284344A1 (en) * | 2016-11-23 | 2019-09-19 | Xiamen University | Preparation method of fluorine-silicon-containing polyphosphate ester and application thereof |
| KR20200001241A (en) * | 2018-06-27 | 2020-01-06 | 듀라원 주식회사 | Waterproofing polyurea resin paints composition for protective explosion and earthquake-proof having flame retardant and preparation method thereof |
| CN117567714A (en) * | 2024-01-18 | 2024-02-20 | 广州市脉田新材料科技有限公司 | Organosilicon hydrophilic flame-retardant finishing agent and preparation method thereof |
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2024
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| US20190284344A1 (en) * | 2016-11-23 | 2019-09-19 | Xiamen University | Preparation method of fluorine-silicon-containing polyphosphate ester and application thereof |
| KR20200001241A (en) * | 2018-06-27 | 2020-01-06 | 듀라원 주식회사 | Waterproofing polyurea resin paints composition for protective explosion and earthquake-proof having flame retardant and preparation method thereof |
| CN117567714A (en) * | 2024-01-18 | 2024-02-20 | 广州市脉田新材料科技有限公司 | Organosilicon hydrophilic flame-retardant finishing agent and preparation method thereof |
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