CN116606442A - Preparation method of sulfonate addition organosilicon flame retardant - Google Patents
Preparation method of sulfonate addition organosilicon flame retardant Download PDFInfo
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- CN116606442A CN116606442A CN202310731169.3A CN202310731169A CN116606442A CN 116606442 A CN116606442 A CN 116606442A CN 202310731169 A CN202310731169 A CN 202310731169A CN 116606442 A CN116606442 A CN 116606442A
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- Prior art keywords
- sulfonate
- flame retardant
- silicon
- siloxane
- unsaturated double
- 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.)
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 50
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 47
- 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 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 28
- 239000001257 hydrogen Substances 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 8
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- -1 methyl hydrogen cyclic siloxane Chemical class 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims description 4
- VAPQAGMSICPBKJ-UHFFFAOYSA-N 2-nitroacridine Chemical compound C1=CC=CC2=CC3=CC([N+](=O)[O-])=CC=C3N=C21 VAPQAGMSICPBKJ-UHFFFAOYSA-N 0.000 claims description 3
- HWDDJFFLFNQAFQ-UHFFFAOYSA-M potassium;4-ethenylbenzenesulfonate Chemical compound [K+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 HWDDJFFLFNQAFQ-UHFFFAOYSA-M 0.000 claims description 3
- SONHXMAHPHADTF-UHFFFAOYSA-M sodium;2-methylprop-2-enoate Chemical compound [Na+].CC(=C)C([O-])=O SONHXMAHPHADTF-UHFFFAOYSA-M 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 2
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 2
- LLLCSBYSPJHDJX-UHFFFAOYSA-M potassium;2-methylprop-2-enoate Chemical compound [K+].CC(=C)C([O-])=O LLLCSBYSPJHDJX-UHFFFAOYSA-M 0.000 claims description 2
- 229940047670 sodium acrylate Drugs 0.000 claims description 2
- 238000007259 addition reaction Methods 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 8
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- JGTNAGYHADQMCM-UHFFFAOYSA-N perfluorobutanesulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F JGTNAGYHADQMCM-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000000655 anti-hydrolysis Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 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
- 229920000642 polymer Polymers 0.000 description 1
- 231100000683 possible toxicity Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/392—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of a sulfonate addition organosilicon flame retardant, which comprises the steps of mixing siloxane containing silicon-hydrogen bonds with an organic solvent to prepare a solution; mixing sulfonate containing unsaturated double bonds with deionized water to prepare an aqueous solution; adding an organic solution containing silicon-hydrogen bond siloxane into a reaction kettle, and controlling the temperature to be in the range of 30-70 ℃; adding a Kanster catalyst into a sulfonate aqueous solution containing unsaturated double bonds, and dropwise adding the solution into a reaction kettle through a dropping pipe; filtering, washing and drying the reaction product to obtain the organic silicon flame retardant; the filtrate was distilled under reduced pressure to recover the organic solvent. The sulfonate containing unsaturated double bond in aqueous solution state and the organic solution containing silicon-hydrogen bond siloxane are subjected to addition reaction under the catalysis of a Karster catalyst, the prepared flame retardant has good compatibility and dispersibility, the heat resistance is greatly improved, the hydrolysis resistance of the sulfonate-added organic silicon flame retardant is excellent, the organic solvent can be recycled, and the whole production process has no pollution to the environment.
Description
Technical Field
The invention relates to the technical field of preparation of organic silicon flame retardants, in particular to a preparation method of a sulfonate addition organic silicon flame retardant.
Background
The phosphate flame retardant is a flame retardant very effective for PC, but has strong internal plasticization effect and has great damage to the mechanical property of the material.
Among the common PC flame retardants, the sulfonate flame retardant has the advantages of small addition amount, good flame retardant property, small molecular weight, poor hydrolysis resistance, poor compatibility and influence on the mechanical property of PC.
Perfluoroalkyl sulfonates and polyfluoroalkyl compounds (pfacs) are widely used in industrial production and life, and perfluorooctyl sulfonate (PFOS) has been disabled and replaced by short-chain pfacs (e.g., perfluorobutyl sulfonate, PFBS) due to its potential toxicity, which is detrimental to animal and human survival; however, some pfases have become a common contaminant in the environment, and thus after the european commission makes decisions according to the proposals of the german and swedish authorities, perfluorinated sulphonic acids and their salts and precursors will be limited in the european/european community of economy since month 2023.
Therefore, it is necessary to develop an anti-hydrolysis, environment-friendly sulfonate-added organic silicon flame retardant for flame retarding PC.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a preparation method of a sulfonate addition organosilicon flame retardant, which comprises the following steps: mixing siloxane containing silicon-hydrogen bond with organic solvent to prepare solution; mixing sulfonate containing unsaturated double bonds with deionized water to prepare an aqueous solution; adding an organic solution containing silicon-hydrogen bond siloxane into a reaction kettle, and controlling the temperature to be in the range of 30-70 ℃; adding a Kanster catalyst into a sulfonate aqueous solution containing unsaturated double bonds, and dropwise adding the solution into a reaction kettle through a dropping pipe; filtering, washing and drying the reaction product to obtain the organic silicon flame retardant; the filtrate was distilled under reduced pressure to recover the organic solvent. Preparing a flame retardant by an addition reaction of a siloxane containing a silicon-hydrogen bond to a sulfonate containing an unsaturated double bond in the presence of a Kanster catalyst; flame retardant PC meets UL94 flame retardant rating.
As an improvement of the sulfonate addition organosilicon flame retardant, the invention intentionally controls the dropping speed when the solution is dropped, avoids the excessively fast dropping speed, accelerates the reaction rate, makes the reaction violently difficult to control, releases heat rapidly too fast and ensures that the flame retardant has uneven particle size; the dripping speed is controlled to ensure the uniformity of the particle size of the product.
In a further technical scheme, the siloxane containing the silicon-hydrogen bond is selected from one or a mixture of more of methyl hydrogen cyclic siloxane, high hydrogen silicone oil and common hydrogen silicone oil.
In a further embodiment, the methylhydrogen cyclic siloxane is selected from the group consisting of D 3 H、D 4 H、D 5 H、D 6 H or a mixture of several of them.
In a further technical scheme, the organic solvent is selected from one or a mixture of more of absolute methanol, absolute ethanol, isopropanol, propylene glycol, butanediol and tetrahydrofuran.
In a further technical scheme, the sulfonate containing unsaturated double bonds is selected from one or a mixture of more of sodium p-styrenesulfonate, potassium p-styrenesulfonate, sodium methacrylate sulfonate, potassium methacrylate sulfonate, sodium acrylate sulfonate and potassium acrylate sulfonate. As an improvement of the invention, the amount of the substance controlling the reactant silicon hydrogen bond exceeds the amount of the substance controlling the sulfonate of unsaturated double bond, and the silicon hydrogen bond has a hydrophobic effect and protects the easy hygroscopicity of the sulfonate.
In a further technical scheme, the weight ratio of the sulfonate containing unsaturated double bonds to the siloxane containing silicon-hydrogen bonds is 8:2-2:8.
In a further technical scheme, the weight ratio of the siloxane containing the silicon-hydrogen bond to the organic solvent is 1:5-5:1. As an improvement of the sulfonate addition organosilicon flame retardant, the organic solvent used in the reaction can be recovered by reduced pressure distillation.
In a further technical scheme, the weight ratio of the sulfonate containing unsaturated double bonds to water is 1:5-1:15.
The sulfonate addition organosilicon flame retardant obtained by the preparation method can be melt blended with PC base materials through double screws for granulation, and the organosilicon structure provides good processability for the polymer.
Compared with the prior art, the invention has the following beneficial technical effects: the sulfonate containing unsaturated double bond and the organic solution containing silicon-hydrogen bond siloxane are subjected to addition reaction under the catalysis of a Karster catalyst, the prepared flame retardant has good compatibility and dispersibility when being applied to PC engineering plastics, the siloxane structure has excellent processability to materials, the heat resistance is greatly improved, meanwhile, the sulfonate addition organic silicon flame retardant has excellent hydrolysis resistance, the production process is simple, the organic solvent can be recycled, the whole production process has no pollution to the environment, and the flame retardant can be used for large-scale industrial production.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention, in order to facilitate the understanding of those skilled in the art.
Example 1
70g to 90g of high hydrogen silicone oil and 150g to 200g of absolute ethyl alcohol are prepared into an alcohol solution, and 30g to 50g of sodium p-styrene sulfonate and 120g to 150g of deionized water are prepared into an aqueous solution; 1 drop of 1000ppm of Kanster catalyst was added dropwise to the aqueous solution; heating the alcohol solution in a reaction kettle, and controlling the reaction temperature to be between 30 and 70 ℃; then adding the aqueous solution into a reaction kettle in a dropwise adding mode; the reaction product is filtered, washed and dried to obtain the organic silicon flame retardant, and the filtrate is distilled under reduced pressure to recover the organic solvent.
Example 2
70 g-90 g D4H and 150 g-200 g absolute methanol are prepared into an alcohol solution, 30 g-50 g potassium p-styrene sulfonate and 120 g-150 g deionized water are prepared into an aqueous solution; 1 drop of 1000ppm of Kanster catalyst was added dropwise to the aqueous solution; the alcohol solution is put into a reaction kettle to be heated, and the reaction temperature is controlled to be 30-70 ℃. Then adding the water solution with the Caster catalyst into a reaction kettle in a dropwise manner; the reaction product is filtered, washed and dried to obtain the organic silicon flame retardant, and the filtrate is distilled under reduced pressure to recover the organic solvent.
Example 3
Preparing organic solution from 40 g-60 g high hydrogen silicone oil and 80 g-120 g tetrahydrofuran, preparing aqueous solution from 60 g-80 g sodium methacrylate sulfonate and 250 g-300 g deionized water; 1 drop of 1000ppm of Kanster catalyst was added dropwise to the above aqueous solution; the organic solution is put into a reaction kettle to be heated, and the reaction temperature is controlled to be 30-70 ℃. Then adding the water solution with the Caster catalyst into a reaction kettle in a dropwise manner; the reaction product is filtered, washed and dried to obtain the organic silicon flame retardant, and the filtrate is distilled under reduced pressure to recover the organic solvent.
Example 4
40g to 60g of high hydrogen silicone oil and 80g to 120g of absolute ethyl alcohol are prepared into an alcohol solution, and 60g to 80g of sodium p-styrene sulfonate and 250g to 300g of deionized water are prepared into an aqueous solution; 1 drop of 1000ppm of Kanster catalyst was added dropwise to the aqueous solution; the alcohol solution is put into a reaction kettle to be heated, and the reaction temperature is controlled to be 30-70 ℃. Then adding the water solution with the Caster catalyst into a reaction kettle in a dropwise manner; the reaction product is filtered, washed and dried to obtain the organic silicon flame retardant, and the filtrate is distilled under reduced pressure to recover the organic solvent.
Example 5
70g to 90g of high hydrogen silicone oil and 150g to 200g of absolute ethyl alcohol are prepared into an alcohol solution, and 30g to 50g of potassium acrylate and 120g to 150g of deionized water are prepared into an aqueous solution; 1 drop of 1000ppm of Kanster catalyst was added dropwise to the aqueous solution; heating the alcohol solution in a reaction kettle, and controlling the reaction temperature to be between 30 and 70 ℃; then adding the water solution with the Caster catalyst into a reaction kettle in a dropwise manner; the reaction product is filtered, washed and dried to obtain the organic silicon flame retardant, and the filtrate is distilled under reduced pressure to recover the organic solvent.
Performance test
Sulfonate-added silicone flame retardants were prepared by the methods of examples 1, 2, 3, 4, and 5 described above, and in order to further illustrate the excellent properties of the flame retardant of the present invention, the sulfonate-added silicone flame retardants and the general sulfonate flame retardants prepared in examples 1 to 5, respectively, were melt-pelletized with PC resin in a twin screw extruder at a ratio of 0.2%. PC resin without flame retardant was pelletized on a twin screw extruder for blank comparison. And then injection molding is carried out on an injection molding machine at a proper temperature to prepare a sample to be tested. The injection molded specimens were tested for UL94 vertical burn testing. The sample was left to stand for 24 hours. The test results are shown in table 1:
TABLE 1UL94 vertical burning test
From table 1 it can be concluded that: the sulfonate-added silicone flame retardant article passed the UL94-V0 flame retardant rating. It can be found from the combination of examples 1 to 5, comparative examples 1 to 2 and Table 1 that: the PC resin added with the sulfonate addition organic silicon flame retardant prepared in any embodiment of the invention has excellent flame retardant property. The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A preparation method of a sulfonate addition organosilicon flame retardant is characterized by comprising the following steps: the method comprises the following steps:
s1: mixing siloxane containing silicon-hydrogen bond with organic solvent to prepare organic solution;
s2: mixing sulfonate containing unsaturated double bonds with deionized water to prepare an aqueous solution;
s3: adding an organic solution containing silicon-hydrogen bond siloxane into a reaction kettle, and controlling the temperature to be in the range of 30-70 ℃;
s4: adding a Kanster catalyst into a sulfonate aqueous solution containing unsaturated double bonds, and dropwise adding the solution into a reaction kettle through a dropping pipe;
s5: filtering, washing and drying the reaction product to obtain the organic silicon flame retardant;
s6: the filtrate was distilled under reduced pressure to recover the organic solvent.
2. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 1, which is characterized in that: the siloxane containing the silicon-hydrogen bond is selected from one or a mixture of a plurality of methyl hydrogen cyclic siloxane, high hydrogen silicone oil and common hydrogen silicone oil.
3. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 2, wherein the method comprises the following steps: the methyl hydrogen cyclic siloxane is selected from D 3 H、D 4 H、D 5 H、D 6 H or a mixture of several of them.
4. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 1, which is characterized in that: the organic solvent is one or a mixture of several of absolute methanol, absolute ethanol, isopropanol, propylene glycol, butanediol and tetrahydrofuran.
5. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 1, which is characterized in that: the sulfonate containing unsaturated double bonds is selected from one or a mixture of more of sodium p-styrenesulfonate, potassium p-styrenesulfonate, sodium methacrylate sulfonate, potassium methacrylate sulfonate, sodium acrylate sulfonate and potassium acrylate sulfonate.
6. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 1, which is characterized in that: the weight ratio of the sulfonate containing unsaturated double bond to the siloxane containing silicon-hydrogen bond is 8:2-2:8.
7. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 1, which is characterized in that: the weight ratio of the siloxane containing the silicon-hydrogen bond to the organic solvent is 1:5-5:1.
8. The method for preparing the sulfonate addition organosilicon flame retardant according to claim 1, which is characterized in that: the weight ratio of the sulfonate containing unsaturated double bonds to water is 1:5-1:15.
9. A sulfonate addition silicone flame retardant obtainable by the process of any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310731169.3A CN116606442A (en) | 2023-06-20 | 2023-06-20 | Preparation method of sulfonate addition organosilicon flame retardant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310731169.3A CN116606442A (en) | 2023-06-20 | 2023-06-20 | Preparation method of sulfonate addition organosilicon flame retardant |
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| CN116606442A true CN116606442A (en) | 2023-08-18 |
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| CN202310731169.3A Pending CN116606442A (en) | 2023-06-20 | 2023-06-20 | Preparation method of sulfonate addition organosilicon flame retardant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117186393A (en) * | 2023-10-11 | 2023-12-08 | 东莞市百富塑料科技有限公司 | Sulfonate flame retardant applied to polycarbonate and synthesis method |
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2023
- 2023-06-20 CN CN202310731169.3A patent/CN116606442A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117186393A (en) * | 2023-10-11 | 2023-12-08 | 东莞市百富塑料科技有限公司 | Sulfonate flame retardant applied to polycarbonate and synthesis method |
| CN117186393B (en) * | 2023-10-11 | 2024-03-29 | 东莞市百富塑料科技有限公司 | Sulfonate flame retardant applied to polycarbonate and synthesis method |
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