CN105153465B - A kind of phosphorus nitrogen silicon compound modified hydrotalcite fire retardant and preparation method thereof - Google Patents
A kind of phosphorus nitrogen silicon compound modified hydrotalcite fire retardant and preparation method thereof Download PDFInfo
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- CN105153465B CN105153465B CN201510653934.XA CN201510653934A CN105153465B CN 105153465 B CN105153465 B CN 105153465B CN 201510653934 A CN201510653934 A CN 201510653934A CN 105153465 B CN105153465 B CN 105153465B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- 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
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Abstract
Description
Claims (7)
- A kind of 1. phosphorus nitrogen silicon compound modified hydrotalcite fire retardant, it is characterised in that phosphorus nitrogen silicon compound modified hydrotalcite fire retardant It is made by following methods:4.6g hydrotalcites are added in 100mL toluene, ultrasonic disperse is moved into after 30 minutes equipped with machinery Stirring, thermometer, reflux condensing tube and dropping funel drying four-hole bottle in, 0.5g 3- propyls are added dropwise at room temperature Oxysilane and 10mL toluene mixture liquids, and rise to reflux temperature, continue to be stirred to react 6 it is small when, be cooled to 30 DEG C, be added dropwise 0.65g diphenyl phosphate chlorides, 2g triethylamines and 15mL toluene mixture liquids, the reaction was continued 4 it is small when;Then slurries obtained by the reaction Filtering, is washed repeatedly with ethyl alcohol, and in 80 DEG C of baking oven it is dry 24 it is small when, it is fire-retardant that phosphorus nitrogen silicon compound modified hydrotalcite is made Agent, the wherein mass content of phosphorus nitrogen silicon compound are 20%.
- A kind of 2. phosphorus nitrogen silicon compound modified hydrotalcite fire retardant, it is characterised in that phosphorus nitrogen silicon compound modified hydrotalcite fire retardant It is made by following methods:2.68g hydrotalcites are added in 50mL toluene, ultrasonic disperse is moved into after 30 minutes equipped with machinery Stirring, thermometer, reflux condensing tube and dropping funel drying four-hole bottle in, 0.5g 3- propyls are added dropwise at room temperature Oxysilane and 10mL toluene mixture liquids, and rise to reflux temperature, continue to be stirred to react 6 it is small when, be cooled to 30 DEG C, be added dropwise 0.65g diphenyl phosphate chlorides, 2g triethylamines and 15mL toluene mixture liquids, the reaction was continued 4 it is small when;Then slurries obtained by the reaction Filtering, is washed repeatedly with ethyl alcohol, and in 80 DEG C of baking oven it is dry 24 it is small when, it is fire-retardant that phosphorus nitrogen silicon compound modified hydrotalcite is made Agent, the wherein mass content of phosphorus nitrogen silicon compound are 30%.
- A kind of 3. phosphorus nitrogen silicon compound modified hydrotalcite fire retardant, it is characterised in that phosphorus nitrogen silicon compound modified hydrotalcite fire retardant It is made by following methods:10.35g hydrotalcites are added in 180mL toluene, ultrasonic disperse is moved into after 30 minutes equipped with machine Tool stirring, thermometer, reflux condensing tube and dropping funel drying four-hole bottle in, 0.5g 3- aminopropyl front threes are added dropwise at room temperature Base oxysilane and 10mL toluene mixture liquids, and rise to reflux temperature, continue to be stirred to react 6 it is small when, be cooled to 30 DEG C, be added dropwise 0.65g diphenyl phosphate chlorides, 2g triethylamines and 15mL toluene mixture liquids, the reaction was continued 4 it is small when;Then slurries obtained by the reaction Filtering, is washed repeatedly with ethyl alcohol, and in 80 DEG C of baking oven it is dry 24 it is small when, it is fire-retardant that phosphorus nitrogen silicon compound modified hydrotalcite is made Agent, the wherein mass content of phosphorus nitrogen silicon compound are 10%.
- A kind of 4. phosphorus nitrogen silicon compound modified hydrotalcite fire retardant, it is characterised in that phosphorus nitrogen silicon compound modified hydrotalcite fire retardant It is made by following methods:113.85g hydrotalcites are added in 1500mL toluene, ultrasonic disperse was moved into and is equipped with after 30 minutes Mechanical agitation, thermometer, reflux condensing tube and dropping funel drying four-hole bottle in, 0.5g 3- aminopropyls three are added dropwise at room temperature Methyl oxysilane and 10mL toluene mixture liquids, and rise to reflux temperature, continue to be stirred to react 6 it is small when, be cooled to 30 DEG C, be added dropwise 0.65g diphenyl phosphate chlorides, 2g triethylamines and 15mL toluene mixture liquids, the reaction was continued 4 it is small when;Then slurries obtained by the reaction Filtering, is washed repeatedly with ethyl alcohol, and in 80 DEG C of baking oven it is dry 24 it is small when, it is fire-retardant that phosphorus nitrogen silicon compound modified hydrotalcite is made Agent, the wherein mass content of phosphorus nitrogen silicon compound are 1%.
- A kind of 5. phosphorus nitrogen silicon compound modified hydrotalcite fire retardant, it is characterised in that phosphorus nitrogen silicon compound modified hydrotalcite fire retardant It is made by following methods:1.725g hydrotalcites are added in 40mL toluene, ultrasonic disperse is moved into after 30 minutes equipped with machinery Stirring, thermometer, reflux condensing tube and dropping funel drying four-hole bottle in, 0.5g 3- propyls are added dropwise at room temperature Oxysilane and 10mL toluene mixture liquids, and rise to reflux temperature, continue to be stirred to react 6 it is small when, be cooled to 30 DEG C, be added dropwise 0.65g diphenyl phosphate chlorides, 2g triethylamines and 15mL toluene mixture liquids, the reaction was continued 4 it is small when;Then slurries obtained by the reaction Filtering, is washed repeatedly with ethyl alcohol, and in 80 DEG C of baking oven it is dry 24 it is small when, it is fire-retardant that phosphorus nitrogen silicon compound modified hydrotalcite is made Agent, the wherein mass content of phosphorus nitrogen silicon compound are 40%.
- 6. a kind of phosphorus nitrogen silicon compound modified hydrotalcite fire retardant described in claim 1 is in terms of flame retardant composite material is prepared Using, it is characterised in that:Phosphorus nitrogen silicon compound modified hydrotalcite fire retardant accounts for the 5-15% of flame retardant composite material gross mass.
- 7. application according to claim 6, it is characterised in that:The flame retardant composite material is modified by phosphorus nitrogen silicon compound Hydrotalcite is with EVA using mass ratio as 9:1 ratio mixes.
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CN105153465A CN105153465A (en) | 2015-12-16 |
CN105153465B true CN105153465B (en) | 2018-05-22 |
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Families Citing this family (5)
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CN109384959B (en) * | 2018-09-11 | 2020-06-09 | 台州职业技术学院 | Preparation method of phosphorus-nitrogen high-load hydrotalcite flame retardant |
CN110157042A (en) * | 2019-04-28 | 2019-08-23 | 北京工商大学 | The application of novel surface inorganic agent, preparation method and the nano particle being processed in resistance combustion polyurethane foam |
CN110305370A (en) * | 2019-06-13 | 2019-10-08 | 湘潭大学 | A kind of phosphonitrile graft modification houghite fire retardant and preparation method thereof |
CN115304636A (en) * | 2022-08-15 | 2022-11-08 | 铨盛聚碳科技股份有限公司 | Organic silicon flame retardant containing phosphorus and nitrogen, and preparation method and application thereof |
CN115385662A (en) * | 2022-09-30 | 2022-11-25 | 广东萨菲安新材料有限公司 | Phosphorus-nitrogen-silicon modified ceramic powder and application thereof |
Citations (4)
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CN101356221A (en) * | 2005-11-08 | 2009-01-28 | 苏普雷斯塔有限责任公司 | Coating compositions for forming inkjet-receptive coatings on a substrate |
CN102757581A (en) * | 2012-07-31 | 2012-10-31 | 华南理工大学 | Intumescent flame retardant functional silicate and preparation method thereof |
CN103387757A (en) * | 2013-07-25 | 2013-11-13 | 北京市建筑工程研究院有限责任公司 | Method for preparing supercritical hydrotalcite grafted with flame retardant |
CN104099055A (en) * | 2013-04-07 | 2014-10-15 | 广东国望精细化学品有限公司 | Halogenn-free flame retardant polyurethane sealant and preparation method thereof |
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CN101356221A (en) * | 2005-11-08 | 2009-01-28 | 苏普雷斯塔有限责任公司 | Coating compositions for forming inkjet-receptive coatings on a substrate |
CN102757581A (en) * | 2012-07-31 | 2012-10-31 | 华南理工大学 | Intumescent flame retardant functional silicate and preparation method thereof |
CN104099055A (en) * | 2013-04-07 | 2014-10-15 | 广东国望精细化学品有限公司 | Halogenn-free flame retardant polyurethane sealant and preparation method thereof |
CN103387757A (en) * | 2013-07-25 | 2013-11-13 | 北京市建筑工程研究院有限责任公司 | Method for preparing supercritical hydrotalcite grafted with flame retardant |
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Application publication date: 20151216 Assignee: ZHEJIANG XINGYU AUTOPARTS Co.,Ltd. Assignor: Taizhou University Contract record no.: 2019330000031 Denomination of invention: Phosphorus-nitrogen-silicon compound modified hydrotalcite flame retardant and preparation method thereof Granted publication date: 20180522 License type: Exclusive License Record date: 20190311 |
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Assignee: ZHEJIANG XINGYU AUTOPARTS Co.,Ltd. Assignor: TAIZHOU University Contract record no.: 2019330000031 Date of cancellation: 20201209 |
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Effective date of registration: 20221212 Address after: 318050 Room 102, building 22, No. 1, Park North Road, fengjiang street, Luqiao District, Taizhou City, Zhejiang Province Patentee after: Zhejiang Longpu Plastic Industry Co.,Ltd. Address before: 1139 Shifu Avenue, Jiaojiang District, Taizhou City, Zhejiang Province Patentee before: TAIZHOU University |