CN100506695C - Method for synthesizing flame retardant of magnesium hydroxide - Google Patents
Method for synthesizing flame retardant of magnesium hydroxide Download PDFInfo
- Publication number
- CN100506695C CN100506695C CNB2007101196067A CN200710119606A CN100506695C CN 100506695 C CN100506695 C CN 100506695C CN B2007101196067 A CNB2007101196067 A CN B2007101196067A CN 200710119606 A CN200710119606 A CN 200710119606A CN 100506695 C CN100506695 C CN 100506695C
- Authority
- CN
- China
- Prior art keywords
- flame retardant
- glutarate
- magnesium hydroxide
- synthesizing
- sodium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 14
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 11
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims description 22
- 239000000347 magnesium hydroxide Substances 0.000 title claims description 22
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 19
- JFCQEDHGNNZCLN-UHFFFAOYSA-N glutaric acid Chemical class OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000006277 sulfonation reaction Methods 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 abstract description 10
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract description 5
- 235000019341 magnesium sulphate Nutrition 0.000 abstract description 5
- 239000003945 anionic surfactant Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000003607 modifier Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000012716 precipitator Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
This invention relates to a method for synthesizing Mg (OH) 2 flame retardant, more specifically, a precipitation method for synthesizing ultrafine Mg (OH) 2 flame retardant. The method comprises: preparing a mixed aqueous solution of MgSO4 (4-18 g/L), NaOH (5-20 g/L) and sulfonated glutarate modifier (0.01-0.03 g/L), and precipitating under microwave to obtain Mg (OH) 2. The particle sizes of Mg (OH) 2 can be decreased by microwave. Different particle sizes (0.1-3 mu.m) of Mg (OH) 2 can be obtained by adjusting the microwave power and time. At the same time, the addition of sulfonated glutarate anionic surfactant can improve the flame retardancy of Mg (OH) 2 flame retardant.
Description
Technical field
The present invention relates to a kind of method for synthesizing flame retardant of magnesium hydroxide, particularly a kind of method that adopts precipitator method synthesizing superfine flame retardant of magnesium hydroxide.
Background technology
Magnesium hydroxide is a kind of application fire retardant very widely, is mainly used in fields such as building, traffic, transportation, electronic apparatus, chemical industry.Find relevant patent CN01134059.2, CN200410067540.8,03134189.6 and 02133360.2, what mainly adopt is the conventional precipitator method and natural brucite preparation, the particle diameter ratio of the magnesium hydroxide of producing is thicker, and granularity is not easy control.
Summary of the invention
The objective of the invention is deficiency, provide a kind of magnesium hydroxide particle diameter of production thin, effectively the method for synthesizing flame retardant of magnesium hydroxide of control size at above-mentioned prior art existence.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method for synthesizing flame retardant of magnesium hydroxide, it is characterized in that its preparation process is to be added with the aqueous solution of sal epsom and sodium hydroxide and properties-correcting agent sulfonation glutarate, after stirring, place microwave reactor, the power of controlling reactor is 100-700W, reaction 15-40min through cooling, filtration, washing, obtains magnesium hydroxide particle then; It is added with in the aqueous solution of sal epsom and sodium hydroxide and properties-correcting agent sulfonation glutarate, and the concentration of sulfur acid magnesium is 4-18g/l, and containing concentration sodium hydroxide is 5-20g/l, and properties-correcting agent sulfonation glutarate add-on is 0.01-0.03g/l.
A kind of method for synthesizing flame retardant of magnesium hydroxide of the present invention utilizes magnesium salts and mineral alkali to make magnesium hydroxide by the microwave precipitation.Its characteristics are to utilize microwave that sedimentary particle is attenuated, control the magnesium hydroxide particle that different microwave powers and time can obtain different-grain diameter, the magnesium hydroxide particle that obtains particle diameter and be 0.1-3 μ m utilizes sulfonation glutarate anion surfactant to make fire retardant usefulness more abundant simultaneously.
Embodiment
A kind of method for synthesizing flame retardant of magnesium hydroxide, its preparation process is to be added with the aqueous solution of sal epsom and sodium hydroxide and properties-correcting agent sulfonation glutarate, the concentration of sulfur acid magnesium is 4-18g/l in the solution, and containing concentration sodium hydroxide is 5-20g/l, and properties-correcting agent sulfonation glutarate amount is 0.01-0.03g/l, after stirring, place microwave reactor, the power of controlling reactor is 100-700W, reaction 15-40min, through cooling, filtration, washing, obtain magnesium hydroxide particle then.
Embodiment 1
At first prepare the magnesium sulfate solution that concentration is 8g/L,, get 200mL in the tetrafluoroethylene cup, adding is with the aqueous sodium hydroxide solution of the 10g/L of volume, and the sulfonation glutarate of 10mL0.5g/L, placing microwave reactor after the stirring rapidly, the power of controlling reactor is 200W, reaction times is 15min, cool off then, filter, with deionized water wash 2 times, 105 ℃ of vacuum-drying 2 hours, observe through SEM, the particle diameter that obtains magnesium hydroxide particle is 2 μ m.
Embodiment 2
At first prepare the magnesium sulfate solution that concentration is 20g/L, get 200mL in the tetrafluoroethylene cup, add aqueous sodium hydroxide solution with the 25g/L of volume, and the sulfonation glutarate of 10mL0.5g/L, place microwave reactor after the stirring rapidly, the power of controlling reactor is 500W, and the reaction times is 20min, cools off then, filters, with deionized water wash 2 times, 105 ℃ of vacuum-drying 2 hours is observed through SEM, and the particle diameter that obtains magnesium hydroxide particle is 1 μ m.
Embodiment 3
At first prepare the magnesium sulfate solution that concentration is 35g/L, get 200mL in the tetrafluoroethylene cup, add aqueous sodium hydroxide solution with the 40g/L of volume, and the sulfonation glutarate of 10mL1g/L, place microwave reactor after the stirring rapidly, the power of controlling reactor is 700W, and the reaction times is 40min, cools off then, filters, with deionized water wash 2 times, 105 ℃ of vacuum-drying 2 hours is observed through SEM, and the particle diameter that obtains magnesium hydroxide particle is 0.2 μ m.
Embodiment 4
At first prepare the magnesium sulfate solution that concentration is 35g/L, get 200mL in the tetrafluoroethylene cup, add aqueous sodium hydroxide solution with the 10g/L of volume, and the sulfonation glutarate of 10mL1g/L, place microwave reactor after the stirring rapidly, the power of controlling reactor is 700W, and the reaction times is 40min, cools off then, filters, with deionized water wash 2 times, 105 ℃ of vacuum-drying 2 hours is observed through SEM, and the particle diameter that obtains magnesium hydroxide particle is 0.4 μ m.
Claims (1)
1. method for synthesizing flame retardant of magnesium hydroxide, it is characterized in that its preparation process is to be added with the aqueous solution of sal epsom and sodium hydroxide and properties-correcting agent sulfonation glutarate, after stirring, place microwave reactor, the power of controlling reactor is 100-700W, reaction 15-40min through cooling, filtration, washing, obtains magnesium hydroxide particle then; It is added with in the aqueous solution of sal epsom and sodium hydroxide and properties-correcting agent sulfonation glutarate, and the concentration of sulfur acid magnesium is 4-18g/l, and containing concentration sodium hydroxide is 5-20g/l, and properties-correcting agent sulfonation glutarate amount is 0.01-0.03g/l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101196067A CN100506695C (en) | 2007-07-27 | 2007-07-27 | Method for synthesizing flame retardant of magnesium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101196067A CN100506695C (en) | 2007-07-27 | 2007-07-27 | Method for synthesizing flame retardant of magnesium hydroxide |
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| Publication Number | Publication Date |
|---|---|
| CN101092241A CN101092241A (en) | 2007-12-26 |
| CN100506695C true CN100506695C (en) | 2009-07-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007101196067A Active CN100506695C (en) | 2007-07-27 | 2007-07-27 | Method for synthesizing flame retardant of magnesium hydroxide |
Country Status (1)
| Country | Link |
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| CN (1) | CN100506695C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160531B (en) * | 2018-11-14 | 2020-11-24 | 绍兴文理学院 | Green preparation method of nano calcium carbonate |
| CN112777617B (en) * | 2021-02-18 | 2022-08-12 | 西部矿业集团有限公司 | Method for preparing magnesium hydroxide for flame retardant by industrial-grade magnesium hydroxide microwave method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1492005A (en) * | 2003-08-29 | 2004-04-28 | 杨治富 | Surface treating coupling agent for natural magnesium hydroxide organic flame-retardant powder |
| CN1513761A (en) * | 2002-12-31 | 2004-07-21 | 浙江大学 | Preparation method of nano-level magnesium hydroxide |
-
2007
- 2007-07-27 CN CNB2007101196067A patent/CN100506695C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513761A (en) * | 2002-12-31 | 2004-07-21 | 浙江大学 | Preparation method of nano-level magnesium hydroxide |
| CN1492005A (en) * | 2003-08-29 | 2004-04-28 | 杨治富 | Surface treating coupling agent for natural magnesium hydroxide organic flame-retardant powder |
Non-Patent Citations (2)
| Title |
|---|
| 氢氧化镁阻燃剂研究进展. 胡章文.轻金属，第7期. 2006 |
| 氢氧化镁阻燃剂研究进展. 胡章文.轻金属，第7期. 2006 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101092241A (en) | 2007-12-26 |
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