CN107459757A - A kind of preparation method and applications of organic-silicon-modified heat-resistant fireproof agent - Google Patents
A kind of preparation method and applications of organic-silicon-modified heat-resistant fireproof agent Download PDFInfo
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- CN107459757A CN107459757A CN201710773325.7A CN201710773325A CN107459757A CN 107459757 A CN107459757 A CN 107459757A CN 201710773325 A CN201710773325 A CN 201710773325A CN 107459757 A CN107459757 A CN 107459757A
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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
- C08L49/00—Compositions of homopolymers or copolymers of compounds having one or more carbon-to-carbon triple bonds; Compositions of derivatives of such polymers
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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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
A kind of preparation method and applications of organic-silicon-modified heat-resistant fireproof agent, belong to technical field of flame retardant.The preparation method comprises the following steps：Epoxy modified silicone resin, poly- aryl ethane resin, water-soluble inorganic film forming matter, dimethylbenzene, cyclohexanone, aluminium hydroxide, titanium dioxide, quartz sand, pentaerythrite, rosin modified phenolic resin and coupling agent are dispersed in ammonia spirit, stirred；It will be heated after mixture grinding after stirring, electric heating synthesis carried out after pressurization；After the completion of reaction, by distillation dehydration, dilution, which is stored in hermetically sealed can, after reactant is cooled down obtains final products.Fire retardant prepared by the present invention, environment-friendly high-efficiency, electrical conductivity is superior, is 35 ~ 45 nS/cm, and beneficial to environment, formaldehydeless, heavy metal component, all raw materials can reclaim cyclic process use.Good with resin compatible, impact strength is good.For high temperature resistant up to more than 720 ~ 800 DEG C, ageing-resistant performance is strong, higher with the construction material such as amalgamation of synthetic rubber, fiber and plastics.
Description
Technical field
The invention belongs to technical field of flame retardant, and in particular to a kind of preparation method of organic-silicon-modified heat-resistant fireproof agent
And its application.
Background technology
Fire retardant, it is a kind of functional aid, combustible polymers can be made fire retardant, primarily directed to the resistance of high polymer material
Combustion design, fire retardant has polytype, is divided into additive flame retardant and reactive flame retardant by application method.Addition property is fire-retardant
Agent is to be added to by the method for mechanical mixture in polymer, polymer is possessed anti-flammability, and adding fire retardant at present mainly has
Organic fire-retardant and inorganic combustion inhibitor, halogenated flame retardant and non-halogen fire retardant.Organic fire-retardant is with bromine system, phosphorus nitrogen system and red phosphorus
And some fire retardants that compound is representative, inorganic combustion inhibitor is mainly the fire retardants such as the antimony of tri-chlorination two, aluminium hydroxide, silicon systems
System.Reactive flame retardant is then to participate in polymerisation as a kind of monomer, polymer is contained flame-retardant composition in itself, its advantage is
Performance influence on polymeric material is smaller, and anti-flammability is lasting.
According to statistics, in the fire incident occurred all over the world, building fire occupy the umber one, is brought to the mankind huge
Loss, most in the every field such as construction material, interior decoration, household furniture, electronic apparatus are various days
Right or synthetic rubber, fiber, plastic or other material, and these high polymer materials are general all inflammable or flammable, this is undoubtedly prevented fire
Calamity occurs and fire-fighting work brings great difficulty, and serious threat the security of the lives and property of the country and people, existing resistance
Less, flame retardant effect also unobvious are applied in combustion agent in terms of construction material.
The content of the invention
The technical problem of solution：For above-mentioned technical problem, the present invention provides a kind of organic-silicon-modified heat-resistant fireproof agent
Preparation method and applications, possess environment-friendly high-efficiency, without pernicious gas, electrical conductivity is superior, high temperature resistant up to more than 800 DEG C,
The advantages that ageing-resistant performance is strong.
Technical scheme：A kind of preparation method of organic-silicon-modified heat-resistant fireproof agent, the preparation method include following step
Suddenly：
（1）By weight, by 0.1 ~ 5 part of epoxy modified silicone resin, 15 ~ 33 parts of poly- aryl ethane resins, 5 ~ 20 parts of water
Insoluble inorganic film forming matter, 3 ~ 6 parts of dimethylbenzene, 2 ~ 7 parts of cyclohexanone, 4 ~ 6 parts of aluminium hydroxides, 3 ~ 5 parts of titanium dioxides, 8 ~ 12 parts of quartz
It is dense that sand, 0.5 ~ 1.5 part of pentaerythrite, 5 ~ 15 parts of rosin modified phenolic resins and 1 ~ 3 part of coupling agent are dispersed in 100 ~ 150 parts of quality
Spend in 30% ~ 60% ammonia spirit, to stir；
（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 30 ~ 50 μm；
（3）To step（2）Middle mixture is heated to 190 ~ 220 DEG C, and electric heating synthesizes under 0.05 ~ 1.5 MPa, reacts 1 ~ 2 h；
（4）After the completion of reaction, by distillation dehydration, by reactant be cooled to 70 ~ 80 DEG C it is standby；
（5）To step（3）It is equal that 4 ~ 6 parts of X-3 Vinylidene Chloride lacquer diluent mixing by weight are added in reactant after cooling
It is even；
（6）By step（5）It is stored in after being sterilized under the mixture uviol lamp of preparation in hermetically sealed can.
Preferably, the step（1）By weight, by 3 parts of epoxy modified silicone resins, 20 parts of poly- aryl ethanes
Resin, 15 parts of water-soluble inorganic film forming matters, 5 parts of dimethylbenzene, 4 parts of cyclohexanone, 5 parts of aluminium hydroxides, 4 parts of titanium dioxides, 10 parts of quartz
It is molten for 45% ammoniacal liquor that sand, 1 part of pentaerythrite, 10 parts of rosin modified phenolic resins and 2 parts of coupling agents are dispersed in 120 parts of mass concentrations
In liquid.
Preferably, the step（1）Middle coupling agent is silane coupler ZQ-560 or Silane coupling agent KH550.
Preferably, the step（5）Middle X-3 Vinylidene Chloride lacquer diluent is stearic acid, zinc stearate or stearic acid
Calcium.
Preferably, the step（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 35 μm.
Preferably, the step（3）It is middle to step（2）Middle mixture is heated to 200 DEG C, and electric heating closes under 0.9 MPa
Into 1.5 h of reaction.
Preferably, the step（4）By reactant be cooled to 80 DEG C it is standby.
Preferably, the step（5）5 parts by weight of X-3 Vinylidene Chloride lacquer diluents are added to be well mixed.
Another technical solution of the present invention is the fire retardant of methods described preparation in construction material such as synthetic rubber, fibre
Application in the modification of peacekeeping plastic flame.
Beneficial effect：Fire retardant prepared by the present invention, environment-friendly high-efficiency, without pernicious gas, electrical conductivity is superior, is 35 ~ 45
NS/cm, beneficial to environment, formaldehydeless, heavy metal component, all raw materials can reclaim cyclic process use.With resin compatible
Good, impact strength is good.For high temperature resistant up to more than 720 ~ 800 DEG C, ageing-resistant performance is strong, with construction material such as synthetic rubber, fiber
It is higher with the amalgamation of plastics.
Embodiment
Embodiment 1
A kind of preparation method of organic-silicon-modified heat-resistant fireproof agent, the preparation method comprise the following steps：
（1）By weight, by 0.1 part of epoxy modified silicone resin, 15 parts of poly- aryl ethane resins, 5 parts of water-soluble inorganics
Film forming matter, 3 parts of dimethylbenzene, 2 parts of cyclohexanone, 4 parts of aluminium hydroxides, 3 parts of titanium dioxides, 8 parts of quartz sands, 0.5 part of pentaerythrite, 5 parts
Rosin modified phenolic resin and 1 part of coupling agent are dispersed in 100 parts of mass concentrations in 60% ammonia spirit, to stir, the idol
Connection agent is silane coupler ZQ-560；
（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 30 μm；
（3）To step（2）Middle mixture is heated to 190 DEG C, and electric heating synthesizes under 0.05 MPa, reacts 1 h；
（4）After the completion of reaction, by distillation dehydration, by reactant be cooled to 70 DEG C it is standby；
（5）To step（3）4 parts of X-3 Vinylidene Chloride lacquer diluents by weight are added in reactant after cooling to be well mixed,
The X-3 Vinylidene Chloride lacquer diluent is stearic acid；
（6）By step（5）It is stored in after being sterilized under the mixture uviol lamp of preparation in hermetically sealed can.
Using fire retardant prepared by the above method answering in construction material such as synthetic rubber, fiber and plastic flame are modified
With.
Fire retardant prepared by the present invention, environment-friendly high-efficiency, without pernicious gas, electrical conductivity is superior, is 45 nS/cm, beneficial to ring
Border, formaldehydeless, heavy metal component, all raw materials can reclaim cyclic process use.Good, the impact strength with resin compatible
It is good.For high temperature resistant up to more than 720 DEG C, ageing-resistant performance is strong, with the construction material such as amalgamation of synthetic rubber, fiber and plastics
It is higher.
Embodiment 2
A kind of preparation method of organic-silicon-modified heat-resistant fireproof agent, the preparation method comprise the following steps：
（1）By weight, by 5 parts of epoxy modified silicone resins, 33 parts of poly- aryl ethane resins, 20 parts of water-soluble inorganics into
Film thing, 6 parts of dimethylbenzene, 7 parts of cyclohexanone, 6 parts of aluminium hydroxides, 5 parts of titanium dioxides, 12 parts of quartz sands, 1.5 parts of pentaerythrites, 15 parts
Rosin modified phenolic resin and 3 parts of coupling agents are dispersed in 150 parts of mass concentrations in 60% ammonia spirit, to stir, the idol
Connection agent is silane coupler ZQ-560.
（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 50 μm.
（3）To step（2）Middle mixture is heated to 220 DEG C, and electric heating synthesizes under 1.5 MPa, reacts 2 h.
（4）After the completion of reaction, by distillation dehydration, by reactant be cooled to 80 DEG C it is standby.
（5）To step（3）6 parts of X-3 Vinylidene Chloride lacquer diluent mixing by weight are added in reactant after cooling
Uniformly, the X-3 Vinylidene Chloride lacquer diluent is zinc stearate.
（6）By step（5）It is stored in after being sterilized under the mixture uviol lamp of preparation in hermetically sealed can.
Using fire retardant prepared by the above method answering in construction material such as synthetic rubber, fiber and plastic flame are modified
With.
Fire retardant prepared by the present invention, environment-friendly high-efficiency, without pernicious gas, electrical conductivity is superior, is 40 nS/cm, beneficial to ring
Border, formaldehydeless, heavy metal component, all raw materials can reclaim cyclic process use.Good, the impact strength with resin compatible
It is good.For high temperature resistant up to more than 750 DEG C, ageing-resistant performance is strong, with the construction material such as amalgamation of synthetic rubber, fiber and plastics
It is higher.
Embodiment 3
A kind of preparation method of organic-silicon-modified heat-resistant fireproof agent, the preparation method comprise the following steps：
（1）By weight, by 3 parts of epoxy modified silicone resins, 20 parts of poly- aryl ethane resins, 15 parts of water-soluble inorganics into
Film thing, 5 parts of dimethylbenzene, 4 parts of cyclohexanone, 5 parts of aluminium hydroxides, 4 parts of titanium dioxides, 10 parts of quartz sands, 1 part of pentaerythrite, 10 portions of pines
Fragrant phenol-formaldehyde resin modified and 2 parts of coupling agents are dispersed in 120 parts of mass concentrations as in 45% ammonia spirit, the coupling agent is silane
Coupling agent KH550.
（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 35 μm.
（3）To step（2）Middle mixture is heated to 200 DEG C, and electric heating synthesizes under 0.9 MPa, reacts 1.5 h.
（4）After the completion of reaction, by distillation dehydration, by reactant be cooled to 80 DEG C it is standby.
（5）To step（3）5 parts of X-3 Vinylidene Chloride lacquer diluent mixing by weight are added in reactant after cooling
Uniformly, the X-3 Vinylidene Chloride lacquer diluent is calcium stearate.
（6）By step（5）It is stored in after being sterilized under the mixture uviol lamp of preparation in hermetically sealed can.
Using fire retardant prepared by the above method answering in construction material such as synthetic rubber, fiber and plastic flame are modified
With.
Fire retardant prepared by the present invention, environment-friendly high-efficiency, without pernicious gas, electrical conductivity is superior, is 35 nS/cm, beneficial to ring
Border, formaldehydeless, heavy metal component, all raw materials can reclaim cyclic process use.Good, the impact strength with resin compatible
It is good.For high temperature resistant up to more than 800 DEG C, ageing-resistant performance is strong, with the construction material such as amalgamation of synthetic rubber, fiber and plastics
It is higher.
Comparative example 1
By step described in embodiment 3（1）Middle aluminium hydroxide and rosin modified phenolic resin change the poly- aryl ethane of homogenous quantities part into
Resin.Remaining step is constant.
After testing, the nS/cm of electrical conductivity 70, good with resin compatible, impact strength is good, and high temperature resistant is up to more than 500 DEG C.
Claims (9)
1. a kind of preparation method of organic-silicon-modified heat-resistant fireproof agent, it is characterised in that the preparation method includes following step
Suddenly：
（1）By weight, by 0.1 ~ 5 part of epoxy modified silicone resin, 15 ~ 33 parts of poly- aryl ethane resins, 5 ~ 20 parts of water
Insoluble inorganic film forming matter, 3 ~ 6 parts of dimethylbenzene, 2 ~ 7 parts of cyclohexanone, 4 ~ 6 parts of aluminium hydroxides, 3 ~ 5 parts of titanium dioxides, 8 ~ 12 parts of quartz
It is dense that sand, 0.5 ~ 1.5 part of pentaerythrite, 5 ~ 15 parts of rosin modified phenolic resins and 1 ~ 3 part of coupling agent are dispersed in 100 ~ 150 parts of quality
Spend in 30% ~ 60% ammonia spirit, to stir；
（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 30 ~ 50 μm；
（3）To step（2）Middle mixture is heated to 190 ~ 220 DEG C, and electric heating synthesizes under 0.05 ~ 1.5 MPa, reacts 1 ~ 2 h；
（4）After the completion of reaction, by distillation dehydration, by reactant be cooled to 70 ~ 80 DEG C it is standby；
（5）To step（3）It is equal that 4 ~ 6 parts of X-3 Vinylidene Chloride lacquer diluent mixing by weight are added in reactant after cooling
It is even；
（6）By step（5）It is stored in after being sterilized under the mixture uviol lamp of preparation in hermetically sealed can.
2. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（1）By weight, by 3 parts of epoxy modified silicone resins, 20 parts of poly- aryl ethane resins, 15 parts of water-soluble inorganics into
Film thing, 5 parts of dimethylbenzene, 4 parts of cyclohexanone, 5 parts of aluminium hydroxides, 4 parts of titanium dioxides, 10 parts of quartz sands, 1 part of pentaerythrite, 10 portions of pines
Fragrant phenol-formaldehyde resin modified and 2 parts of coupling agents are dispersed in 120 parts of mass concentrations as in 45% ammonia spirit.
3. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（1）Middle coupling agent is silane coupler ZQ-560 or Silane coupling agent KH550.
4. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（5）Middle X-3 Vinylidene Chloride lacquer diluent is stearic acid, zinc stearate or calcium stearate.
5. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（2）Mixture after stirring is put into mill paint machine and is ground to fineness as 35 μm.
6. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（3）It is middle to step（2）Middle mixture is heated to 200 DEG C, and electric heating synthesizes under 0.9 MPa, reacts 1.5 h.
7. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（4）By reactant be cooled to 80 DEG C it is standby.
8. the preparation method of a kind of organic-silicon-modified heat-resistant fireproof agent according to claim 1, it is characterised in that described
Step（5）5 parts by weight of X-3 Vinylidene Chloride lacquer diluents are added to be well mixed.
9. changed based on fire retardant prepared by claim 1 methods described in construction material such as synthetic rubber, fiber and plastic flame
Application in property.
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| CN201710773325.7A CN107459757A (en) | 2017-08-31 | 2017-08-31 | A kind of preparation method and applications of organic-silicon-modified heat-resistant fireproof agent |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432920A (en) * | 2011-08-17 | 2012-05-02 | 中科院广州化学有限公司 | High-temperature-resistant nuclear-shell structure type flame retardant, and preparation method and application thereof |
| CN105295049A (en) * | 2015-12-04 | 2016-02-03 | 江苏涌新材料科技有限公司 | Halogen-free environment-friendly synergistic organic silicon flame retardant, flame retardant composition as well as preparation method and application of synergistic organic silicon flame retardant |
-
2017
- 2017-08-31 CN CN201710773325.7A patent/CN107459757A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432920A (en) * | 2011-08-17 | 2012-05-02 | 中科院广州化学有限公司 | High-temperature-resistant nuclear-shell structure type flame retardant, and preparation method and application thereof |
| CN105295049A (en) * | 2015-12-04 | 2016-02-03 | 江苏涌新材料科技有限公司 | Halogen-free environment-friendly synergistic organic silicon flame retardant, flame retardant composition as well as preparation method and application of synergistic organic silicon flame retardant |
Non-Patent Citations (1)
| Title |
|---|
| 余瑞莲等: "聚芳基乙炔树脂基复合材料复合工艺研究", 《复合材料——基础、创新、高效：第十四届全国复合材料学术会议论文集（上）》 * |
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