CN108840344A - A kind of preparation method of magnesium silicon series composite flame retardant - Google Patents
A kind of preparation method of magnesium silicon series composite flame retardant Download PDFInfo
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- CN108840344A CN108840344A CN201810805574.4A CN201810805574A CN108840344A CN 108840344 A CN108840344 A CN 108840344A CN 201810805574 A CN201810805574 A CN 201810805574A CN 108840344 A CN108840344 A CN 108840344A
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- silica
- flame retardant
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/155—Preparation of hydroorganogels or organogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
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- Materials Engineering (AREA)
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- Fireproofing Substances (AREA)
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Abstract
The invention discloses a kind of preparation method of magnesium silicon series composite flame retardant, the preparation method includes the following steps：(1) ethyl orthosilicate of certain mol proportion is added to absolute ethanol, is stirred evenly, acid solution is added dropwise, adjusting pH value is 6.0~6.5, and 30~40min is stirred under 50~60 DEG C of water bath conditions, obtains silica solution；(2) alkaline solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.1~7.5, add it is a certain amount of crossed through ball milling, partial size be 100~300nm magnesium hydroxide particle and silica dioxide granule, 30~40min of ultrasonic disperse, it mixes them thoroughly uniformly, obtains the silica solution containing magnesium hydroxide and silica；(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash, it is dry, obtain magnesium silicon series composite flame retardant.Magnesium silicon series composite flame retardant preparation method in the present invention is simple, fire retardant controllable size and appearance, good dispersion.
Description
Technical field
The present invention relates to technical field of flame retardant, more particularly to a kind of preparation method of magnesium silicon series composite flame retardant.
Background technique
In recent years, for protection environment and human life and health the considerations of and American-European countries make halogen system organic fire-retardant
Stringent limitation, the research of environmental-friendly inorganic fire retardants, production and application situation are extremely urgent.China's magnesium abundant
Resource makes Domestic Magnesium Hydroxide Flame Retardant have wide research and prospect of production, and development potentiality is huge.
From last century the nineties, people begin to focus on flame retardant of magnesium hydroxide, and foreign countries have gradually formed industrialization, state
Inside also have and has largely been reported about magnesium fire-retardant agent.It is mostly raw material, precipitating-hydro-thermal method using magnesite, brine or seawater
Sheet, acicular magnesium hydroxide is prepared；Also have and react simultaneously water with alkali using basic magnesium chloride, boric magnesium fertilizer, alkali magnesium sulfate etc.
Heat treatment obtains magnesium hydroxide crystal whisker, fiber or nanotube；Magnesia hydration is prepared magnesium hydroxide by also useful hydro-thermal method.It is close
Year, the research of magnesium hydroxide composite fire retardant is paid attention to.But there are preparation process complexity, obtained resistance for the above method
Fire the undesirable problem of agent dispersibility.
For this reason, it is necessary to be able to solve in view of the above-mentioned problems, propose a kind of preparation method of magnesium silicon series composite flame retardant
Problems of the prior art.
Summary of the invention
It is in the prior art to overcome the purpose of the present invention is to provide a kind of preparation method of magnesium silicon series composite flame retardant
It is insufficient.
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of magnesium silicon series composite flame retardant, the preparation method include the following steps：
(1) ethyl orthosilicate of certain mol proportion is added to absolute ethanol, is stirred evenly, acid solution is added dropwise, adjusted
PH value is 6.0~6.5, and 30~40min is stirred under 50~60 DEG C of water bath conditions, obtains silica solution；
(2) alkaline solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.1~7.5, is added a certain amount of
It is crossed through ball milling, the magnesium hydroxide particle and silica dioxide granule that partial size is 100~300nm, 30~40min of ultrasonic disperse makes it
It is sufficiently mixed uniformly, obtains the silica solution containing magnesium hydroxide and silica；
(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash
It washs, it is dry, obtain magnesium silicon series composite flame retardant.
Preferably, in step (1), the molar ratio of the ethyl orthosilicate and the dehydrated alcohol is 1:2~4.
Preferably, in step (1), the acid solution is hydrochloric acid solution.
Preferably, in step (2), the alkaline solution is ammonia spirit.
Preferably, in step (2), the molar ratio of the magnesium hydroxide particle and the silica dioxide granule is 3~8:1.
Preferably, the molar ratio of the magnesium hydroxide particle and the silica dioxide granule is 5:1.
Preferably, in step (2), 50~100g magnesium hydroxide particle and silica are contained in every 500g silica solution
Grain.
Preferably in step (3), drying temperature is 110~150 DEG C.
Compared with the prior art, the advantages of the present invention are as follows：Magnesium silicon series composite flame retardant preparation method letter in the present invention
It is single, fire retardant controllable size and appearance, good dispersion.
Specific embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of magnesium silicon series composite flame retardant, and the preparation method includes the following steps：
(1) ethyl orthosilicate of certain mol proportion is added to absolute ethanol, is stirred evenly, acid solution is added dropwise, adjusted
PH value is 6.0~6.5, and 30~40min is stirred under 50~60 DEG C of water bath conditions, obtains silica solution；
(2) alkaline solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.1~7.5, is added a certain amount of
It is crossed through ball milling, the magnesium hydroxide particle and silica dioxide granule that partial size is 100~300nm, 30~40min of ultrasonic disperse makes it
It is sufficiently mixed uniformly, obtains the silica solution containing magnesium hydroxide and silica；
(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash
It washs, it is dry, obtain magnesium silicon series composite flame retardant.
Wherein, in step (1), the molar ratio of the ethyl orthosilicate and the dehydrated alcohol is 1:2~4, it is preferred that institute
The molar ratio for stating ethyl orthosilicate and the dehydrated alcohol is 1:3；The acid solution is hydrochloric acid solution；It is described in step (2)
Alkaline solution is ammonia spirit；The molar ratio of the magnesium hydroxide particle and the silica dioxide granule is 3~8:1, it is preferred that
The molar ratio of the magnesium hydroxide particle and the silica dioxide granule is 5:1.
Following preparation methods that the magnesium silicon series composite flame retardant in the present invention is illustrated with specifically embodiment.
Embodiment 1
It (1) is 1 by certain mol proportion:2 ethyl orthosilicate is added to absolute ethanol, and is stirred evenly, and hydrochloric acid solution is added dropwise,
Adjusting pH value is 6.0, stirs 30min under 50 DEG C of water bath conditions, obtains silica solution；
(2) ammonia aqueous solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.1, and adding molar ratio is 3:
1, it is crossed through ball milling, the magnesium hydroxide particle and silica dioxide granule that partial size is 100nm, ultrasonic disperse 30min is mixed them thoroughly
Uniformly, the silica solution containing magnesium hydroxide and silica is obtained, wherein contain 50g magnesium hydroxide in every 500g silica solution
Grain and silica dioxide granule；
(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash
It washs, it is dry at a temperature of 110 DEG C, obtain magnesium silicon series composite flame retardant.
Embodiment 2
It (1) is 1 by certain mol proportion:3 ethyl orthosilicate is added to absolute ethanol, and is stirred evenly, and hydrochloric acid solution is added dropwise,
Adjusting pH value is 6.2, stirs 35min under 55 DEG C of water bath conditions, obtains silica solution；
(2) ammonia aqueous solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.3, and adding molar ratio is 5:
1, it is crossed through ball milling, the magnesium hydroxide particle and silica dioxide granule that partial size is 200nm, ultrasonic disperse 35min is mixed them thoroughly
Uniformly, the silica solution containing magnesium hydroxide and silica is obtained, wherein contain 80g magnesium hydroxide in every 500g silica solution
Grain and silica dioxide granule；
(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash
It washs, it is dry at a temperature of 130 DEG C, obtain magnesium silicon series composite flame retardant.
Embodiment 3
It (1) is 1 by certain mol proportion:4 ethyl orthosilicate is added to absolute ethanol, and is stirred evenly, and hydrochloric acid solution is added dropwise,
Adjusting pH value is 6.5, stirs 40min under 50~60 DEG C of water bath conditions, obtains silica solution；
(2) ammonia aqueous solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.5, and adding molar ratio is 8:
1, it is crossed through ball milling, the magnesium hydroxide particle and silica dioxide granule that partial size is 300nm, ultrasonic disperse 40min is mixed them thoroughly
Uniformly, the silica solution containing magnesium hydroxide and silica is obtained, wherein contain 100g magnesium hydroxide in every 500g silica solution
Grain and silica dioxide granule；
(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash
It washs, it is dry at a temperature of 150 DEG C, obtain magnesium silicon series composite flame retardant.
It is real that UL94 vertical combustion is carried out to the magnesium silicon series composite flame retardant that the method in above-described embodiment 1~3 is prepared
It tests, the results showed that, the magnesium silicon series composite flame retardant that the method in above-described embodiment 1~3 is prepared does not occur molten drop phenomenon,
Thus illustrate that the magnesium silicon series composite flame retardant has good flame retardant property.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (8)
1. a kind of preparation method of magnesium silicon series composite flame retardant, which is characterized in that the preparation method includes the following steps：
(1) ethyl orthosilicate of certain mol proportion is added to absolute ethanol, is stirred evenly, acid solution is added dropwise, adjust pH value
It is 6.0~6.5,30~40min is stirred under 50~60 DEG C of water bath conditions, obtains silica solution；
(2) alkaline solution is added dropwise into above-mentioned silica solution, the pH value for adjusting solution is 7.1~7.5, is added a certain amount of through ball
Honed, partial size is the magnesium hydroxide particle and silica dioxide granule of 100~300nm, and 30~40min of ultrasonic disperse makes it sufficiently
It is uniformly mixed, obtains the silica solution containing magnesium hydroxide and silica；
(3) dispersing agent is added into the above-mentioned silica solution containing magnesium hydroxide and silica, stirs evenly, filter, wash, do
It is dry, obtain magnesium silicon series composite flame retardant.
2. magnesium silicon series composite flame retardant according to claim 1, which is characterized in that in step (1), the ethyl orthosilicate
Molar ratio with the dehydrated alcohol is 1:2~4.
3. magnesium silicon series composite flame retardant according to claim 1, which is characterized in that in step (1), the acid solution is
Hydrochloric acid solution.
4. magnesium silicon series composite flame retardant according to claim 1, which is characterized in that in step (2), the alkaline solution is
Ammonia spirit.
5. magnesium silicon series composite flame retardant according to claim 1, which is characterized in that in step (2), the magnesium hydroxide
The molar ratio of grain and the silica dioxide granule is 3~8:1.
6. magnesium silicon series composite flame retardant according to claim 5, which is characterized in that the magnesium hydroxide particle and described two
The molar ratio of silicon oxide particle is 5:1.
7. magnesium silicon series composite flame retardant according to claim 1, which is characterized in that in step (2), in every 500g silica solution
Contain 50~100g magnesium hydroxide particle and silica dioxide granule.
8. magnesium silicon series composite flame retardant according to claim 1, which is characterized in that in step (3), drying temperature 110
~150 DEG C.
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| CN201810805574.4A CN108840344A (en) | 2018-07-20 | 2018-07-20 | A kind of preparation method of magnesium silicon series composite flame retardant |
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| CN201810805574.4A CN108840344A (en) | 2018-07-20 | 2018-07-20 | A kind of preparation method of magnesium silicon series composite flame retardant |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505025A (en) * | 2018-11-27 | 2019-03-22 | 华叶莹 | A kind of anti-fire modified PET fiber and preparation method thereof |
| WO2020140389A1 (en) * | 2019-01-06 | 2020-07-09 | 微山宏瑞电力科技有限公司 | Pure inorganic covering flame-retardant fireproof high-temperature-resistant coating additive and preparation method therefor |
| CN111926934A (en) * | 2020-07-20 | 2020-11-13 | 甘肃巴斯得建筑节能材料科技有限公司 | Preparation method of composite flame retardant for fireproof heat-insulation decorative board |
-
2018
- 2018-07-20 CN CN201810805574.4A patent/CN108840344A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505025A (en) * | 2018-11-27 | 2019-03-22 | 华叶莹 | A kind of anti-fire modified PET fiber and preparation method thereof |
| WO2020140389A1 (en) * | 2019-01-06 | 2020-07-09 | 微山宏瑞电力科技有限公司 | Pure inorganic covering flame-retardant fireproof high-temperature-resistant coating additive and preparation method therefor |
| CN111926934A (en) * | 2020-07-20 | 2020-11-13 | 甘肃巴斯得建筑节能材料科技有限公司 | Preparation method of composite flame retardant for fireproof heat-insulation decorative board |
| CN111926934B (en) * | 2020-07-20 | 2022-03-15 | 甘肃坤远节能环保科技发展有限公司 | Preparation method of composite flame retardant for fireproof heat-insulation decorative board |
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