CN102491381A - Preparation method for flame retardant magnesium hydroxide - Google Patents
Preparation method for flame retardant magnesium hydroxide Download PDFInfo
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- CN102491381A CN102491381A CN2011104218134A CN201110421813A CN102491381A CN 102491381 A CN102491381 A CN 102491381A CN 2011104218134 A CN2011104218134 A CN 2011104218134A CN 201110421813 A CN201110421813 A CN 201110421813A CN 102491381 A CN102491381 A CN 102491381A
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- magnesium hydroxide
- flame retardant
- magnesium
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- scrubbing
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Abstract
The invention discloses a preparation method for flame retardant magnesium hydroxide, which includes: a, dissolving: dissolving magnesium ionic compound into aqueous solution to generate magnesium ion contained solution; b, precipitation/reaction: adding precipitating agent into filtered magnesium ionic solution to generate magnesium hydroxide and then precipitating; c, filtering: filtering precipitate to obtain magnesium hydroxide; d, scrubbing: scrubbing the filtered magnesium hydroxide, wherein the scrubbing includes forepart mother liquid scrubbing and later impurity scrubbing, the forepart mother liquid scrubbing is used for scrubbing entrained mother liquid and uses normal water as scrubbing solution which can be recovered for dissolving magnesium salt at the step a, and the later impurity scrubbing is used for scrubbing impurities entrained by precipitate and soluble impurities and uses deionized water with electric conductivity smaller than 0.2mS/m as scrubbing solution; e, repulping, adding a certain quality of water into filtered magnesium hydroxide for repulping to obtain magnesium hydroxide slurry of a certain mass fraction; and f, grinding: grinding the magnesium hydroxide slurry in a zirconia circulative ball mill. Finished flame retardant magnesium hydroxide produced by the preparation method is higher in impurity and proper in particle size distribution.
Description
Technical field
The present invention relates to chemical field, particularly a kind of flame retardant of magnesium hydroxide preparation method.
Background technology
Because fire is very big for the harm of people's security of the lives and property, therefore, fire preventing, it is very important to reduce the fire possibility occurrence.Wherein, superpolymer being carried out fire-retardant finish then is one of important measures that reduce fire.
Fire retardant is the flame retardancy that can improve inflammable or combustible matl, stops material to be ignited and suppresses a kind of important auxiliary agent of propagation of flame, causes fire easily solving macromolecular material, guarantees that the security aspect that synthetic materials uses plays an important role.
Flame retardant of magnesium hydroxide is one of most widely used kind in the halogen-free flame retardants.Because Marinco H is in fire-retardant; Also, be widely used in plastics, elastomerics and the elastomeric materials such as SE (PVC), Vestolen PP 7052 (PP), Vilaterm (PE), vinyl acetate (EVA), PS (PS), polyamide (PA) with pressing down cigarette, high thermal stability, efficiently promoting base material to become characteristics such as charcoal effect and deacidification ability.The ideal flame retardant of magnesium hydroxide adds in the polymkeric substance and to require to have higher purity and suitable size-grade distribution.Because Marinco H needs higher loading level as fire retardant; If the particle of used Marinco H is bigger; Add prepared matrix material in the matrix to; Between Marinco H and matrix, form crackle easily, thereby influence the overall performance of material, and the purity of Marinco H is again the determinative of matrix material electric property.
Brucite is natural Marinco H, can obtain the flame retardant products of granularity in required scope through wet grinding.But because natural brucite purity is lower, foreign matter contents such as iron, calcium are higher, add the decline that tends to cause the matrix material electric property in the macromolecular material to as fire retardant.
Summary of the invention
In order to solve the problems referred to above of prior art, be necessary to provide a kind of flame retardant of magnesium hydroxide preparation method with higher degree and better size-grade distribution.
The technical scheme that technical solution problem of the present invention provides is: a kind of flame retardant of magnesium hydroxide preparation method,
Comprise the steps:
A, dissolving is dissolved formation with the mg ion compound and is contained magnesium ion solution in the aqueous solution;
B, precipitation/reaction, the magnesium ion solution after filtering adds precipitation agent, and the generation Marinco H also precipitates;
C filters, and filtering precipitate obtains Marinco H;
D, washing, the Marinco H behind the washing and filtering; Wherein, Specifically comprise washing of leading portion mother liquor and the washing of back segment impurity; Wherein the washing of leading portion mother liquor is used to wash the mother liquor of carrying secretly; Its washings adopts ortho-water and can continue to reclaim and is used for step a and dissolves magnesium salts, and the washing of back segment impurity is used to wash impurity and the soluble impurity that settling is carried secretly, adopt specific conductivity less than the deionized water of 0.2mS/m as washings;
E, slurry adds certain water gaging with the Marinco H after filtering and starches processing more again, is made into certain mass fractional Marinco H slurry;
F grinds, and the Marinco H slurry is in zirconic circulation grinding in ball grinder.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method; Also comprise step a1 between step a and the step b: filter, filter, also comprise step g after the step f: drying to containing magnesium ion solution; Magnesium hydroxide particle to after grinding carries out drying, obtains flame retardant of magnesium hydroxide.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, the precipitation agent among the step b can be an ammoniacal liquor, a kind of in sodium hydroxide or the milk of lime, and the washings after the washing of steps d posterior segment impurity also can continue on for the mother liquor washing.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, the flame retardant of magnesium hydroxide purity for preparing is greater than 99%, cl content＜0.05%, and iron level＜100ppm, particle diameter is at 0.5-3 μ m, and specific surface area is at 5-10m
2/ g.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, being made into solid content when starching is the Marinco H slip of 10%-60% again.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, the flame retardant of magnesium hydroxide particle diameter of preparation is 1.2 μ m, and specific surface area is 8.2m
2/ g.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, the flame retardant of magnesium hydroxide particle diameter of preparation is 2.3 μ m, and specific surface area is 5.1m
2/ g.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, said mg ion compound is a kind of in magnesium chloride or the sal epsom.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, zirconic diameter described in the step f is 1-3mm, and milling time is 30-240 minute.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, comprise further among the step f that adding proportion that weight accounts for the Marinco H solid content is 0.01%～0.1% dispersion agent.
Among the above-mentioned flame retardant of magnesium hydroxide preparation method, the dispersion agent among the step f is a polyacrylate.
Compared to prior art, flame retardant of magnesium hydroxide preparation method of the present invention comprises in the solution that contains mg ion and adds precipitation agent, through the control reasonable process conditions; Comprise precipitation/reaction; Washing is filtered etc., obtain the higher magnesium hydroxide products of purity after; Obtain the magnesium hydroxide products of perfect condition again through wet grinding, can prepare the flame retardant of magnesium hydroxide that satisfies the demands with high purity and suitable particle size.
Description of drawings
Fig. 1 is the schematic flow sheet of flame retardant of magnesium hydroxide preparation method one embodiment of the present invention;
Embodiment
Below in conjunction with accompanying drawing the present invention is described further.
Embodiment 1
Seeing also Fig. 1, is the schematic flow sheet of an embodiment of flame retardant of magnesium hydroxide preparation method of the present invention.Said flame retardant of magnesium hydroxide preparation method comprises:
Step S1, dissolving contains magnesium ion solution with the mg ion compound dissolution in heated in water solution formation;
Step S2 filters, and the magnesium ion solution that contains that obtains among the step S1 is filtered;
Step S3, precipitation/reaction, the magnesium ion solution after filtering adds precipitation agent, and the generation Marinco H also precipitates;
Step S4 filters, and filtering precipitate obtains Marinco H;
Step S5, washing, the Marinco H behind the washing and filtering; Specifically comprise washing of leading portion mother liquor and the washing of back segment impurity; Wherein mother liquor washing adopts ortho-water get final product, mainly is the mother liquor (soluble magnesium salts solution) that washing is carried secretly, and its washings can continue recovery and be used for step S1 and dissolve magnesium salts.Impurity and soluble impurity that the main washing of impurity washing settling is carried secretly, it adopts the washings of predefined specific conductivity repeatedly to wash.In the present embodiment, needs use specific conductivity is repeatedly washed less than the deionized water (zero(ppm) water) of 0.2mS/m (every meter milli siemens).Washings after the impurity washing also can continue on for the mother liquor washing.
Step S6, slurry adds certain water gaging with the Marinco H after filtering and starches processing more again, is made into certain mass fractional Marinco H slurry;
Step S7 grinds, and the Marinco H slurry is obtained magnesium hydroxide particle at the grinding machine for grinding certain hour;
Step S8, drying is carried out drying to the magnesium hydroxide particle after grinding, and is met the flame retardant of magnesium hydroxide product that parameter needs.
In embodiment according to the invention and other embodiment, step 2 can be omitted, and precipitation agent described in the step S3 can adopt ammoniacal liquor, sodium hydroxide, milk of lime etc., the milling time among the step S7 be 30-240min (minute).
Embodiment 2
In another embodiment of the present invention, comprise step:
Dissolving is dissolved in sal epsom in the aqueous solution;
Filter, obtain the Adlerika that concentration is 1.9M;
Precipitation/reaction is got the Adlerika that 300ml concentration is 1.9M, heat to 70 ℃ (degree centigrade) after, add the ammoniacal liquor of 2mol/L with the flow of 60ml/min, control reaction end pH value is within 8-10;
Filter, filtering precipitate obtains Marinco H;
Washing is repeatedly washed the magnesium hydrate precipitate thing with the zero(ppm) water of 60 ℃ specific conductivity less than 0.2mS/m, promptly gets purity greater than 99%, cl content＜0.05%, iron level＜100ppm, the high purity magnesium hydroxide product of particle diameter about 1.2 μ m;
Slurry is got a certain amount of high purity magnesium hydroxide again, adds a certain amount of water and starches processing again, is made into massfraction greater than 40% Marinco H slip;
Grinding, is the zirconic circulation grinding in ball grinder of 1-1.2mm 60min at diameter;
Drying, promptly getting particle diameter is 2.3 μ m, specific surface area is 5.1m
2The magnesium hydroxide products of/g.
Embodiment 3
In another embodiment of the present invention, comprise step:
Dissolving is dissolved in magnesium chloride in the aqueous solution;
Filter, obtain the magnesium chloride solution that concentration is 2.84mol/L;
Precipitation/reaction; After in the reactor drum of 2L, adding 500mL zero(ppm) water heat temperature raising to 65 ℃, add above-mentioned magnesium chloride solution, add the ammoniacal liquor of 6.72mol/L simultaneously with the flow of 5ml/min with the flow of 6ml/min; Time is 51min, and entire reaction course pH value remains in the scope of 8-10;
Filter, filtering precipitate obtains Marinco H;
Washing is repeatedly washed the magnesium hydrate precipitate thing with the zero(ppm) water of specific conductivity less than 0.2mS/m, promptly gets purity greater than 99%, cl content＜0.05%, iron level＜100ppm, the high purity magnesium hydroxide of particle diameter about 7 μ m;
Slurry is got a certain amount of high purity magnesium hydroxide again, adds a certain amount of water and starches processing again, and being made into solid content is the Marinco H slip of 10%-60%;
Grinding, is the zirconic circulation grinding in ball grinder of 1-3mm 90min at diameter;
Drying, promptly getting particle diameter is 1.2 μ m, specific surface area is 8.2m
2The magnesium hydroxide products of/g.
In other embodiments of the present invention, precipitation agent can be an ammoniacal liquor, a kind of in sodium hydroxide or the milk of lime, and the washings after the washing of back segment impurity also can continue on for the mother liquor washing.Milling time in the grinding steps is 30-240 minute, and can to add proportion that weight accounts for the Marinco H solid content be 0.01%～0.1% dispersion agent.Said dispersion agent can be a polyacrylate.
In sum, flame retardant of magnesium hydroxide preparation method of the present invention comprises in the solution that contains mg ion and adds precipitation agent, through the control reasonable process conditions; Comprise precipitation/reaction, washing is filtered etc.; After obtaining the higher magnesium hydroxide products of purity, obtain the magnesium hydroxide products of perfect condition again through wet grinding, can prepare the flame retardant of magnesium hydroxide that satisfies the demands with high purity and suitable particle size; For example, add the wet method polishing through chemosynthesis of the present invention and can obtain product purity＞99.0%, cl content＜0.05%; Iron level＜100ppm, particle diameter is in the 0.5-3 mu m range simultaneously, and specific surface area is at 5-10m
2Flame retardant of magnesium hydroxide product in the/g scope.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, can also make some simple deduction or replace, all should be regarded as belonging to protection scope of the present invention.
Claims (13)
1. a flame retardant of magnesium hydroxide preparation method is characterized in that, comprises the steps:
A, dissolving is dissolved formation with the mg ion compound and is contained magnesium ion solution in the aqueous solution;
B, precipitation/reaction, the magnesium ion solution after filtering adds precipitation agent, and the generation Marinco H also precipitates;
C filters, and filtering precipitate obtains Marinco H;
D, washing, the Marinco H behind the washing and filtering; Wherein, Specifically comprise washing of leading portion mother liquor and the washing of back segment impurity; Wherein the washing of leading portion mother liquor is used to wash the mother liquor of carrying secretly; Its washings adopts ortho-water and can continue to reclaim and is used for step a and dissolves magnesium salts, and the washing of back segment impurity is used to wash impurity and the soluble impurity that settling is carried secretly, adopt specific conductivity less than the deionized water of 0.2mS/m as washings;
E, slurry adds certain water gaging with the Marinco H after filtering and starches processing more again, is made into certain mass fractional Marinco H slurry;
F grinds, and the Marinco H slurry is in zirconic circulation grinding in ball grinder.
2. flame retardant of magnesium hydroxide preparation method according to claim 1 is characterized in that, also comprises step a1 between step a and the step b: filter, filter containing magnesium ion solution; Also comprise step g after the step f: drying, the magnesium hydroxide particle after grinding is carried out drying, obtain flame retardant of magnesium hydroxide.
3. flame retardant of magnesium hydroxide preparation method according to claim 2 is characterized in that, the precipitation agent among the step b can be an ammoniacal liquor, a kind of in sodium hydroxide or the milk of lime.
4. flame retardant of magnesium hydroxide preparation method according to claim 2 is characterized in that, the washings after the washing of steps d posterior segment impurity also can continue on for the mother liquor washing.
5. flame retardant of magnesium hydroxide preparation method according to claim 3 is characterized in that, the flame retardant of magnesium hydroxide purity for preparing is greater than 99%, cl content＜0.05%, and iron level＜100ppm, particle diameter is at 0.5-3 μ m, and specific surface area is at 5-10m
2/ g.
6. flame retardant of magnesium hydroxide preparation method according to claim 5 is characterized in that, being made into solid content when starching is the Marinco H slip of 10%-60% again.
7. flame retardant of magnesium hydroxide preparation method according to claim 6 is characterized in that, the flame retardant of magnesium hydroxide particle diameter of preparation is 1.2 μ m, and specific surface area is 8.2m
2/ g.
8. flame retardant of magnesium hydroxide preparation method according to claim 6 is characterized in that, the flame retardant of magnesium hydroxide particle diameter of preparation is 2.3 μ m, and specific surface area is 5.1m
2/ g.
9. according to the arbitrary described flame retardant of magnesium hydroxide preparation method of claim 1-8, it is characterized in that said mg ion compound is a kind of in magnesium chloride or the sal epsom.
10. according to the arbitrary described flame retardant of magnesium hydroxide preparation method of claim 1-8, it is characterized in that among the step f, said zirconic diameter is 1-3mm.
11. flame retardant of magnesium hydroxide preparation method according to claim 10 is characterized in that, among the step f, milling time is 30-240 minute.
12. according to the arbitrary described flame retardant of magnesium hydroxide preparation method of claim 1-8, it is characterized in that, among the step f, comprise that further adding proportion that weight accounts for the Marinco H solid content is 0.01%～0.1% dispersion agent.
13. flame retardant of magnesium hydroxide preparation method according to claim 12 is characterized in that, used dispersion agent is a polyacrylate.
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| CN201110421813.4A CN102491381B (en) | 2011-12-16 | 2011-12-16 | Preparation method for flame retardant magnesium hydroxide |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665939A (en) * | 2013-12-27 | 2014-03-26 | 江苏艾特克阻燃材料有限公司 | Method for integrally preparing high-dispersity ultrafine magnesium hydroxide flame retardant |
| CN105073867A (en) * | 2013-02-19 | 2015-11-18 | 神岛化学工业株式会社 | Flame retardant agent, flame-retardant composition, and molded article |
| CN106115748A (en) * | 2016-06-16 | 2016-11-16 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN109705396A (en) * | 2018-12-11 | 2019-05-03 | 江苏艾特克阻燃材料有限公司 | A kind of magnesium hydroxide composite fire retardant and preparation method thereof for polyamide |
| CN110790549A (en) * | 2019-11-18 | 2020-02-14 | 泉州市派腾新材料科技有限公司 | Preparation method of composite fireproof coating for tunnel |
| CN112574758A (en) * | 2020-12-28 | 2021-03-30 | 江苏聚千新材料科技有限公司 | Heat-conducting flame retardant and preparation process thereof |
| CN113150377A (en) * | 2020-10-16 | 2021-07-23 | 南通意特化工有限公司 | Preparation method of magnesium hydroxide flame retardant |
| CN113980490A (en) * | 2021-11-16 | 2022-01-28 | 江西广源化工有限责任公司 | Magnesium hydroxide with high specific surface area, and preparation method and application thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109810487A (en) * | 2019-01-24 | 2019-05-28 | 中山市绿浪助剂有限公司 | Heat-resistant plastic |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105073867A (en) * | 2013-02-19 | 2015-11-18 | 神岛化学工业株式会社 | Flame retardant agent, flame-retardant composition, and molded article |
| CN103665939A (en) * | 2013-12-27 | 2014-03-26 | 江苏艾特克阻燃材料有限公司 | Method for integrally preparing high-dispersity ultrafine magnesium hydroxide flame retardant |
| CN104592790A (en) * | 2013-12-27 | 2015-05-06 | 江苏艾特克阻燃材料有限公司 | Method for controlling and modifying grain diameter of magnesium hydrate |
| CN104592789B (en) * | 2013-12-27 | 2018-12-04 | 江苏艾特克阻燃材料有限公司 | A kind of preparation method of flame retardant of magnesium hydroxide |
| CN106115748A (en) * | 2016-06-16 | 2016-11-16 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN106115748B (en) * | 2016-06-16 | 2018-01-09 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN109705396A (en) * | 2018-12-11 | 2019-05-03 | 江苏艾特克阻燃材料有限公司 | A kind of magnesium hydroxide composite fire retardant and preparation method thereof for polyamide |
| CN110790549A (en) * | 2019-11-18 | 2020-02-14 | 泉州市派腾新材料科技有限公司 | Preparation method of composite fireproof coating for tunnel |
| CN113150377A (en) * | 2020-10-16 | 2021-07-23 | 南通意特化工有限公司 | Preparation method of magnesium hydroxide flame retardant |
| CN112574758A (en) * | 2020-12-28 | 2021-03-30 | 江苏聚千新材料科技有限公司 | Heat-conducting flame retardant and preparation process thereof |
| CN113980490A (en) * | 2021-11-16 | 2022-01-28 | 江西广源化工有限责任公司 | Magnesium hydroxide with high specific surface area, and preparation method and application thereof |
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| CN102491381B (en) | 2014-06-25 |
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Effective date of registration: 20200818 Address after: No.11, Gandong 3rd road, Ganhe Industrial Park, Xining City, Qinghai Province Patentee after: Qinghai aitek Salt Lake Technology Co., Ltd Address before: Gaocheng Town, Jiangsu city of Yixing province is 214214 Road No. 68 Patentee before: ATK FLAME RETARDANT MATERIALS Co. |
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