CN103980713A - Preparation method of antimony-free high environment-friendly fire retardant mixture and antimony-free high environment-friendly fire retardant mixture - Google Patents
Preparation method of antimony-free high environment-friendly fire retardant mixture and antimony-free high environment-friendly fire retardant mixture Download PDFInfo
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Abstract
The invention discloses an antimony-free high environment-friendly fire retardant mixture and a preparation method. The mixture is prepared from the following crude components in parts by weight: 180-230 parts of a magnesium-aluminum inorganic fire retardant, 0.5-2 parts of a titanate coupling agent, 250-300 parts of a phosphate liquid fire retardant, 200-250 parts of an organic silicon fire retardant, 70-100 parts of melamine, 90-120 parts of cyanuric acid, 600-1000 parts of de-ionized water and 7-50 parts of a fire-retardance synergist. The preparation method comprises the following steps: firstly, implementing surface treatment on the magnesium-aluminum inorganic fire retardant through the titanate coupling agent; then, preparing a melamine-cyanuric acid microcapsule inorganic fire retardant from the surface-treated magnesium-aluminum inorganic fire retardant, the de-ionized water, the fire-retardance synergist, the melamine and the cyanuric acid through a microencapsulation technology; finally, preparing the antimony-free high environment-friendly fire retardant mixture from the phosphate liquid fire retardant, the organic silicon fire retardant and the melamine-cyanuric acid microcapsule inorganic fire retardant through a spraying mixing technology.
Description
Technical field
The present invention relates to fire retardant manufacturing technology field, be specifically related to a kind of integrate process for treating surface, microcapsule treatment technology, low speed constant temperature stir spray compound treatment technology not containing the preparation method of antimony high-environmental flame-retardant mixture and containing antimony high-environmental flame-retardant mixture.
Background technology
Along with the development of city's economic construction and the raising of people's living standard, fire retardant material has been widely used in every field.According to ASSOCIATE STATISTICS data, show, only 2012, Chinese fire retardant material market demand reached 2,300 hundred million yuan, and wherein the growth rate of demand of electric wire aspect reaches 58%.Strategic new industry be take as main in Shenzhen, comprises that people's livelihood science and technology waits other industries, along with whole city's rapid development of economy, to the demand of fire retardant material aspect also lifting just year by year.Under this prerequisite, be accompanied by constantly perfecting and carrying out and implementing of fire retardant material relevant laws and regulations and standard, every profession and trade will stricter to the application of fire retardant material with screening, but to quantize demand larger simultaneously.
At present, bromide fire retardant, because of its excellent cost performance, ranks first of each based flame retardant its market scale and Application Areas for a long time, and the city's applied fire retardant material of each industry also be take this based flame retardant interpolation mixture as main.Yet, along with the enhancing of people's environmental consciousness, bromide fire retardant because of produce and use procedure in the environmental hazard that may cause be under suspicion, European Union, from 1 day July in 2006, in electronic product field, stops using bromide fire retardant.The economic construction in the city and social development are all carried out around the theme of " environmental protection and Sustainable development ", only because the research and development technology of city's field of new fire retardant material slowly fails to reform at present, so far still do not have a kind of with high content of technologyly and meet the product of city's Economic development trend demand, fire retardant material research and development technology circumstances urgently changes.
Development in science and technology is maked rapid progress, and Sb system fire retardant, because itself and the chlorine atom in polyvinyl chloride molecular chain exist good synergistic effect, adds and can reach good flame retardant effect on a small quantity, is subject in recent years industry and favors.But the fire-retardant raw cigarette amount of antimony-chlorine flame-retardant system is high, easily fire-retardant, and weisspiessglanz dust has larger harm to respiratory system, can not meet the demand of the city to flame retardant products.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of not containing the preparation method of antimony high-environmental flame-retardant mixture and not containing antimony high-environmental flame-retardant mixture of addressing the above problem.
The present invention addresses the above problem the technical scheme adopting to be:
, containing a preparation method for antimony high-environmental flame-retardant mixture, it does not specifically comprise the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
Magnesium-aluminium in described step (1) is inorganic combustion inhibitor, and it is a kind of or and the combination in magnesium hydroxide, aluminium hydroxide or magnesium aluminum-hydrotalcite.
Phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n is selected from the even number between 1,3 or 2～18;
X is selected from Cl, Br, PF
6or N (CF
3sO
2)
2.
Silicone flame retardant in described step (1), it is a kind of liquid or and combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
Retardant synergist in described step (1), it is a kind of and combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
Adopt above-mentioned containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
Described magnesium-aluminium is inorganic combustion inhibitor, and it is a kind of or and the combination in magnesium hydroxide, aluminium hydroxide or magnesium aluminum-hydrotalcite.
Described phosphoric acid ester liquid flame retardant, its structural formula is:
R=C in formula
nh
2n+1, n is selected from the even number between 1,3 or 2～18;
X is selected from Cl, Br, PF
6or N (CF
3sO
2)
2.
Described silicone flame retardant, it is a kind of liquid or and combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
Described retardant synergist, it is a kind of and combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
The present invention uses nontoxic, low cigarette, low corrosion and cheap inorganic combustion inhibitor---magnesium-aluminium system, phosphoric acid system and silicone flame retardant, traditional antimony-halogen flame retardant system is converted to the flame-proof environmental protection system that does not contain antimony class, and utilize the process for treating surface in international forward position, low speed constant temperature stirs sprinkling compound treatment technology multiple fire retardant is carried out to compound processing, reaches environmental protection flame retardant object.
Disclosed by the invention not containing antimony high-environmental fire retardant material, can improve that traditional polyvinyl chloride wire cable material use range is little, the easy defect such as migration of winter hardiness, weather resistance, antioxidant deficiency and softening agent, improve synergistic effect and dispersing uniformity between each fire retardant, strengthen the bonding force between itself and polyvinyl chloride, solved inorganic combustion inhibitor modification affect pvc material mechanical property technical barrier.
Below in conjunction with accompanying drawing and embodiment, the present invention is further described.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the present invention;
Embodiment
Embodiment 1:
Referring to Fig. 1, the invention provides a kind of preparation method who does not contain antimony high-environmental flame-retardant mixture, it specifically comprises the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
Magnesium-aluminium in described step (1) is inorganic combustion inhibitor, and it is a kind of or and the combination in magnesium hydroxide, aluminium hydroxide or magnesium aluminum-hydrotalcite.
Phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n is selected from the even number between 1,3 or 2～18;
X is selected from Cl, Br, PF
6or N (CF
3sO
2)
2.
Silicone flame retardant in described step (1), it is a kind of liquid or and combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
Retardant synergist in described step (1), it is a kind of and combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
Adopt above-mentioned containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
Described magnesium-aluminium is inorganic combustion inhibitor, and it is a kind of or and the combination in magnesium hydroxide, aluminium hydroxide or magnesium aluminum-hydrotalcite.
Described phosphoric acid ester liquid flame retardant, its structural formula is:
R=C in formula
nh
2n+1, n is selected from the even number between 1,3 or 2～18;
X is selected from Cl, Br, PF
6or N (CF
3sO
2)
2.
Described silicone flame retardant, it is a kind of liquid or and combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
Described retardant synergist, it is a kind of and combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
Embodiment 2:
What the present embodiment provided does not contain the preparation method of antimony high-environmental flame-retardant mixture and does not contain antimony high-environmental flame-retardant mixture, and its basal component and step are all identical with embodiment 1, and its difference is:
, containing a preparation method for antimony high-environmental flame-retardant mixture, it does not specifically comprise the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 8min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 300 revs/min, temperature is under the condition of 30 ℃, stir 20min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 80 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 150 ℃ of temperature, stirring reaction is 1.5 hours, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 100um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1.5h, obtain not containing antimony high-environmental flame-retardant mixture.
Magnesium-aluminium in described step (1) is inorganic combustion inhibitor, and it is magnesium aluminum-hydrotalcite.
Phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n=3;
X is PF
6.
Silicone flame retardant in described step (1), it is polydimethyl diethoxy silane.
Retardant synergist in described step (1), it is dipentaerythrityl ether.
Adopt above-mentioned containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 8min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 300 revs/min, temperature is under the condition of 30 ℃, stir 20min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 80 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 150 ℃ of temperature, stirring reaction is 1.5 hours, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 100um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 1.5h, obtain not containing antimony high-environmental flame-retardant mixture.
Embodiment 3:
What the present embodiment provided does not contain the preparation method of antimony high-environmental flame-retardant mixture and does not contain antimony high-environmental flame-retardant mixture, and its basal component and step are all identical with embodiment 1,2, and its difference is:
, containing a preparation method for antimony high-environmental flame-retardant mixture, it does not specifically comprise the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 250 revs/min, temperature is under the condition of 30 ℃, stir 25min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 110 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 90 ℃ of temperature, stirring reaction is 1 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 75 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1h, obtain not containing antimony high-environmental flame-retardant mixture.
Magnesium-aluminium in described step (1) is inorganic combustion inhibitor, and it is the combination of magnesium hydroxide, aluminium hydroxide.
Phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n=4;
X is N (CF
3sO
2)
2.
Silicone flame retardant in described step (1), it is the combination of methyl phenyl silicone resin, polyphenyl methoxylsilane.
Retardant synergist in described step (1), it is the combination of phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane.
Adopt above-mentioned containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 250 revs/min, temperature is under the condition of 30 ℃, stir 25min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 110 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 90 ℃ of temperature, stirring reaction is 1 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 75 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 1h, obtain not containing antimony high-environmental flame-retardant mixture.
Embodiment 4:
What the present embodiment provided does not contain the preparation method of antimony high-environmental flame-retardant mixture and does not contain antimony high-environmental flame-retardant mixture, and its basal component and step are all identical with embodiment 1,2,3, and its difference is:
, containing a preparation method for antimony high-environmental flame-retardant mixture, it does not specifically comprise the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
Magnesium-aluminium in described step (1) is inorganic combustion inhibitor, and it is the combination of magnesium hydroxide, aluminium hydroxide, magnesium aluminum-hydrotalcite.
Phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n=2;
X is Cl.
Silicone flame retardant in described step (1), it is the combination of methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane.
Retardant synergist in described step (1), its be phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, combination.
Adopt above-mentioned containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 10min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 400 revs/min, temperature is under the condition of 30 ℃, stir 30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 150 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 200 ℃ of temperature, stirring reaction is 2 hours, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 300um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 2h, obtain not containing antimony high-environmental flame-retardant mixture.
Embodiment 5:
What the present embodiment provided does not contain the preparation method of antimony high-environmental flame-retardant mixture and does not contain antimony high-environmental flame-retardant mixture, and its basal component and step are all identical with embodiment 1,2,3,4, and its difference is:
, containing a preparation method for antimony high-environmental flame-retardant mixture, it does not specifically comprise the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 7min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 335 revs/min, temperature is under the condition of 30 ℃, stir 27min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 125 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 175 ℃ of temperature, stirring reaction is 1.6 hours, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 165um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 75 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1.6h, obtain not containing antimony high-environmental flame-retardant mixture.
Magnesium-aluminium in described step (1) is inorganic combustion inhibitor, and it is the combination of aluminium hydroxide, magnesium aluminum-hydrotalcite.
Phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n=18;
X is Br.
Silicone flame retardant in described step (1), it is the combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
Retardant synergist in described step (1), it is the combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
Adopt above-mentioned containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 7min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 335 revs/min, temperature is under the condition of 30 ℃, stir 27min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 125 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 175 ℃ of temperature, stirring reaction is 1.6 hours, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 165um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 75 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 1.6h, obtain not containing antimony high-environmental flame-retardant mixture.
The present invention is described in more details technical scheme of the present invention by above-mentioned specific embodiment, but the present invention is not limited to the embodiment of above-mentioned proposition.Can not be interpreted as the restriction of protection domain of the present invention, the person skilled in the art in this field can make corresponding improvement and adjustment to the present invention according to foregoing invention content.
The present invention uses nontoxic, low cigarette, low corrosion and cheap inorganic combustion inhibitor---magnesium-aluminium system, phosphoric acid system and silicone flame retardant, traditional antimony-halogen flame retardant system is converted to the flame-proof environmental protection system that does not contain antimony class, and utilize the process for treating surface in international forward position, low speed constant temperature stirs sprinkling compound treatment technology multiple fire retardant is carried out to compound processing, reaches environmental protection flame retardant object.
Disclosed by the invention not containing antimony high-environmental fire retardant material, can improve that traditional polyvinyl chloride wire cable material use range is little, the easy defect such as migration of winter hardiness, weather resistance, antioxidant deficiency and softening agent, improve synergistic effect and dispersing uniformity between each fire retardant, strengthen the bonding force between itself and polyvinyl chloride, solved inorganic combustion inhibitor modification affect pvc material mechanical property technical barrier.
The present invention is not limited to above-mentioned embodiment, adopt raw material and the preparation method identical or approximate with the above embodiment of the present invention, and other similar ink used for plastic that obtain is all within protection scope of the present invention.
Claims (10)
1. not containing a preparation method for antimony high-environmental flame-retardant mixture, it is characterized in that: it specifically comprises the steps:
(1) raw-material preparation
According to following parts by weight, prepare starting material:
(2) magnesium-aluminium is the surface treatment of inorganic combustion inhibitor
Magnesium-aluminium that step (1) is prepared is that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds step (1) to prepare, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
(3) preparation of melamine cyanuric acid microcapsule inorganic frame retardant
By the magnesium-aluminium after step (2) surface treatment, it is inorganic combustion inhibitor, the deionized water of preparing in step (1) adds belt stirrer, in the reactor of thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add the retardant synergist of preparing in step (1), trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, after pulverizing, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um,
(4) low speed constant temperature sprays and stirs compound processing
First, phosphoric acid ester liquid flame retardant, the silicone flame retardant step (1) prepared carry out premix, secondly, the melamine cyanuric acid microcapsule inorganic frame retardant that step (3) is prepared joins in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, by pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joins in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, dry, after granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
2. according to claim 1 not containing the preparation method of antimony high-environmental flame-retardant mixture, it is characterized in that: the magnesium-aluminium in described step (1) is inorganic combustion inhibitor, it is a kind of or and the combination in magnesium hydroxide, aluminium hydroxide or magnesium aluminum-hydrotalcite.
3. according to claim 1 not containing the preparation method of antimony high-environmental flame-retardant mixture, it is characterized in that: the phosphoric acid ester liquid flame retardant in described step (1), its structural formula is:
R=C in formula
nh
2n+1, n is selected from the even number between 1,3 or 2～18;
X is selected from Cl, Br, PF
6or N (CF
3sO
2)
2.
4. according to claim 1 not containing the preparation method of antimony high-environmental flame-retardant mixture, it is characterized in that: the silicone flame retardant in described step (1), it is a kind of liquid or and combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
5. according to claim 1 not containing the preparation method of antimony high-environmental flame-retardant mixture, it is characterized in that: the retardant synergist in described step (1), it is a kind of and combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
6. adopt one of claim 1～5 containing the preparation method of antimony high-environmental flame-retardant mixture, do not prepare not containing an antimony high-environmental flame-retardant mixture, it is characterized in that: it is prepared according to following parts by weight by following composition of raw materials component:
Wherein said is not to prepare by following method containing antimony high-environmental flame-retardant mixture:
First, by the magnesium-aluminium of preparation, be that inorganic combustion inhibitor packs surface preparation device into and stirs, heats after preheating 5～10min, the titanate coupling agent that adds preparation, at stirring rod rotating speed, it is 250～400 revs/min, temperature is under the condition of 30 ℃, stir 20～30min, obtaining surface treated magnesium-aluminium is inorganic combustion inhibitor;
Secondly, by the magnesium-aluminium after surface treatment, be that inorganic combustion inhibitor, deionized water add in the reactor of belt stirrer, thermometer, under the condition of 80～150 ℃ of temperature, make it to disperse, then add retardant synergist, trimeric cyanamide and cyanuric acid, under the condition of 90～200 ℃ of temperature, stirring reaction is 1～2 hour, until obtain white or light cream or thickness paste, by white or light cream or thickness paste after filtration or centrifugation, dry, pulverize after, obtain the melamine cyanuric acid microcapsule inorganic frame retardant of 0.01-300um;
Finally, first phosphoric acid ester liquid flame retardant, silicone flame retardant are carried out to premix; Again melamine cyanuric acid microcapsule inorganic frame retardant is joined in the horizontal mixer of temperature controlling heating, described horizontal mixer, it comprises a cylinder cap, described cylinder cap is provided with a flusher, pre-mixed phosphoric acid ester liquid flame retardant, silicone flame retardant mixed solution joined in flusher, constant temperature 10 ℃ of temperature, under the condition that stirring velocity is 50～100 revs/min, carry out the synergistic blend of inorganic environment-friendly fire retardant and organic environmental-protection fire retardant, after dry, granulation, stir after 1～2h, obtain not containing antimony high-environmental flame-retardant mixture.
7. the antimony high-environmental flame-retardant mixture that do not contain according to claim 6, is characterized in that: described magnesium-aluminium is inorganic combustion inhibitor, and it is a kind of or and the combination in magnesium hydroxide, aluminium hydroxide or magnesium aluminum-hydrotalcite.
8. according to claim 6 not containing antimony high-environmental flame-retardant mixture, it is characterized in that: described phosphoric acid ester liquid flame retardant, its structural formula is:
R=C in formula
nh
2n+1, n is selected from the even number between 1,3 or 2～18;
X is selected from Cl, Br, PF
6or N (CF
3sO
2)
2.
9. according to claim 6 not containing antimony high-environmental flame-retardant mixture, it is characterized in that: described silicone flame retardant, it is a kind of liquid or and combination in methyl phenyl silicone resin, polyphenyl methoxylsilane, poly-dimethoxydiphenylsilane or polydimethyl diethoxy silane.
10. according to claim 6 not containing antimony high-environmental flame-retardant mixture, it is characterized in that: described retardant synergist, it is a kind of and combination in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, dipentaerythrityl ether.
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| CN111378215A (en) * | 2020-04-29 | 2020-07-07 | 嘉兴学院 | Halogen-free flame retardant and preparation method thereof |
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| CN113912909A (en) * | 2021-10-21 | 2022-01-11 | 扬州工业职业技术学院 | Melamine cyanurate/LDH composite flame-retardant material and preparation method thereof |
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| CN116462559A (en) * | 2023-05-09 | 2023-07-21 | 浏阳象形精品烟花出口制造有限公司 | Novel safe and environment-friendly smokeless colloid spray anther |
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| CN110077067A (en) * | 2019-03-12 | 2019-08-02 | 常州斯威克光伏新材料有限公司 | Anti- polarization type EVA compound cutan of double-layer coextrusion and preparation method thereof |
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| CN113912909A (en) * | 2021-10-21 | 2022-01-11 | 扬州工业职业技术学院 | Melamine cyanurate/LDH composite flame-retardant material and preparation method thereof |
| CN114714460A (en) * | 2022-04-15 | 2022-07-08 | 何菊 | Shaving board and preparation method thereof |
| CN114714460B (en) * | 2022-04-15 | 2022-11-18 | 何菊 | Shaving board and preparation method thereof |
| CN116462559A (en) * | 2023-05-09 | 2023-07-21 | 浏阳象形精品烟花出口制造有限公司 | Novel safe and environment-friendly smokeless colloid spray anther |
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