CN113620323A - A kind of preparation method of flame retardant magnesium hydroxide - Google Patents
A kind of preparation method of flame retardant magnesium hydroxide Download PDFInfo
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- CN113620323A CN113620323A CN202110941370.5A CN202110941370A CN113620323A CN 113620323 A CN113620323 A CN 113620323A CN 202110941370 A CN202110941370 A CN 202110941370A CN 113620323 A CN113620323 A CN 113620323A
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- flame retardant
- magnesium hydroxide
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- filtered
- magnesium oxide
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- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 27
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 27
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 26
- 239000003063 flame retardant Substances 0.000 title claims abstract description 22
- 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 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 22
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 22
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002699 waste material Substances 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 11
- 239000011777 magnesium Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 6
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229910001447 ferric ion Inorganic materials 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229920006351 engineering plastic Polymers 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 6
- 238000001556 precipitation Methods 0.000 abstract description 2
- 229910019440 Mg(OH) Inorganic materials 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 159000000003 magnesium salts Chemical class 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001448 ferrous ion Inorganic materials 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000003738 black carbon Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- 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
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
本发明公开了一种阻燃剂氢氧化镁的制备方法：取氧化镁废弃物，研磨粉碎、煅烧，将剩余固体加入盐酸中进行酸溶，过滤溶液，产生沉淀；在过滤出的溶液中，搅拌条件下加入H2O2，使溶液由绿色变为黄色，沉淀、过滤，将过滤后的溶液逐滴滴加氨水，调配pH值，生成的沉淀为Mg(OH)2，过滤干燥。本发明对硅钢级氧化镁进行回收利用，使得环境的压力减少了，是一种较为绿色环保的阻燃剂氢氧化镁制备方案。The invention discloses a preparation method of flame retardant magnesium hydroxide: taking magnesium oxide waste, grinding, pulverizing and calcining, adding the remaining solid into hydrochloric acid for acid dissolution, filtering the solution to produce precipitation; in the filtered solution, Add H 2 O 2 under stirring to make the solution change from green to yellow, precipitate and filter, add ammonia water dropwise to the filtered solution to adjust pH value, the resulting precipitate is Mg(OH) 2 , which is filtered and dried. The invention recycles and utilizes silicon steel grade magnesium oxide, so that the pressure of the environment is reduced, and is a relatively green and environment-friendly preparation scheme of the flame retardant magnesium hydroxide.
Description
Technical Field
The invention relates to a preparation method and application of magnesium hydroxide used for preparing a flame retardant from silicon steel grade magnesium oxide, and belongs to the technical field of recycling of silicon steel grade magnesium oxide.
Background
In recent years, many serious fires have been associated with polymer materials. High molecular materials are used in large quantities due to their characteristics of low cost, easy processing, good formability, low specific gravity, and the like. Therefore, research on flame retardancy of polymer materials has also been urgently conducted.
The quality of the oriented silicon steel is improved by the imported silicon steel grade magnesium oxide in a factory, and a large amount of waste is caused by the high value-added product while the product competitiveness is improved. Meanwhile, the market demands fire-retardant grade magnesium hydroxide and other magnesium salt products are vigorous, and the magnesium hydroxide is an environment-friendly fire retardant. Therefore, the technology for recycling the magnesium oxide waste not only accords with the current national industrial policies of energy conservation, emission reduction and sustainable development, but also has huge market potential of magnesium hydroxide and good economic benefit.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to utilize magnesium oxide waste to produce the magnesium hydroxide reduces the market price of the magnesium oxide.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of flame retardant magnesium hydroxide comprises the following steps:
step 1): taking magnesium oxide waste, grinding, crushing, putting into a crucible, calcining at 600 ℃, and reacting carbon in the magnesium oxide waste with oxygen in the air to generate CO2Weighing the residual solid;
step 2): adding the rest solid into hydrochloric acid for acid dissolution, and adding Mg in the waste2+And Fe2+Then the reaction is carried out, the solution is filtered, and the generated precipitate is impurities;
step 3): adding H into the filtered solution under stirring2O2Changing the solution from green to yellow, i.e. Fe2+Conversion to Fe3+Precipitating, filtering, and filtering to obtain yellow solid Fe3+；
Step 4): dropwise adding ammonia water into the filtered solution, adjusting the pH value, and obtaining a precipitate Mg (OH)2And filtering and drying.
Preferably, the calcination time in step 1) is 6h, and then carbon and oxygen completely react, and ferrous ions are partially oxidized into ferric ions, so as to facilitate later removal.
Preferably, the molar ratio of the magnesium oxide to the hydrochloric acid in the residual solid in the step 2) is 1:2-2.25, and the acid dissolution mode is stirring in a water bath at 60 ℃ for 5 hours.
Preferably, the impurities in step 2) comprise SiO2And unreacted C.
Preferably, H is added in the step 3)2O2The pH of the solution was then 8.5.
Preferably, PEG is added to the solution filtered in the step 4) in addition to ammonia water, so that Mg (OH) obtained by precipitation can be obtained2The size is thinner.
The process route provided by the invention can ensure that 100% of resources of magnesium oxide waste for oriented silicon steel are recycled, the process route for preparing flame-retardant grade magnesium hydroxide from the magnesium oxide waste is obtained, and the key technology and process for preparing the flame-retardant grade magnesium hydroxide from the magnesium oxide waste are mastered.
The invention also provides application of the flame retardant magnesium hydroxide prepared by the preparation method of the flame retardant magnesium hydroxide in ultrahigh engineering plastic composite materials.
Preferably, the flame retardant magnesium hydroxide and the ultra-high molecular weight polyethylene are prepared into the filter through a sintering process. The filter can resist the temperature of 80-160 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. large-area waste magnesium oxide does not need to be re-buried, so that the treatment cost of industrial waste is reduced;
2. the waste industrial waste residue is recycled, so that the environment is protected;
3. the market price of the magnesium oxide can be reduced by utilizing the magnesium hydroxide produced by the magnesium oxide waste.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
Examples
A preparation method of flame retardant magnesium hydroxide comprises the following steps:
1) and (3) calcining to remove carbon: calcining magnesium oxide waste gas in a muffle furnace at 600 ℃ for 2h to remove impurities such as black carbon, and reacting carbon with oxygen in air to generate CO in the heating process2Meanwhile, slurry components organic matters in the waste also undergo the reaction; the metal oxides in the waste are further oxidized to higher oxides, such as oxygenThe ferrous oxide is oxidized to ferric oxide. The process can achieve the carbon removal effect, activate the waste and facilitate the subsequent acid dissolution experiment.
2) Acid dissolution to form crude magnesium salts: the magnesium oxide is dissolved by using hydrochloric acid with the concentration of 6mol/L as a dissolving agent under the condition of stirring at 60 ℃, and finally, crude magnesium salt containing more impurities, particularly high iron content is generated, and the dissolving time is controlled to be 1 h.
3) Purification of crude magnesium salts high purity magnesium salts: compressed air and ammonia water are introduced into the solution to oxidize part of ferrous ions in the solution into ferric ions, which is beneficial to Fe (OH)3Is Fe with a pH of 93+Complete sedimentation, and Mg (OH)2No sedimentation occurred, and the reaction time in this case was preferably controlled to 45 min.
4)Mg(OH)2Generation of (1): to promote flaky Mg (OH)2Adding a surfactant and ethanol into the solution, controlling the concentration of ammonia water to be 1 wt% ammonia water and 5 wt% ethanol solution, allowing the generated magnesium hydroxide to flow out from the bottom of a sedimentation tank, and allowing the supernatant of the sedimentation tank to be used as a fertilizer material.
Claims (8)
1. The preparation method of the flame retardant magnesium hydroxide is characterized by comprising the following steps:
step 1): taking magnesium oxide waste, grinding, crushing, putting into a crucible, calcining at 600 ℃, and reacting carbon in the magnesium oxide waste with oxygen in the air to generate CO2Weighing the residual solid;
step 2): adding the rest solid into hydrochloric acid for acid dissolution, and adding Mg in the waste2+And Fe2+Then the reaction is carried out, the solution is filtered, and the generated precipitate is impurities;
step 3): adding H into the filtered solution under stirring2O2Changing the solution from green to yellow, i.e. Fe2+Conversion to Fe3+Precipitating, filtering, and filtering to obtain yellow solid Fe3+；
Step 4): dropwise adding the filtered solutionAdding ammonia water, adjusting pH value, and obtaining Mg (OH) as precipitate2And filtering and drying.
2. The method for preparing magnesium hydroxide as a flame retardant of claim 1, wherein the calcination time in the step 1) is 2 to 6 hours.
3. The method for preparing magnesium hydroxide as a flame retardant according to claim 1, wherein the molar ratio of magnesium oxide to hydrochloric acid in the remaining solid in the step 2) is 1:2-2.25, and the acid-soluble form is stirring in a water bath at 60 ℃ for 5 hours.
4. The method for preparing magnesium hydroxide as a flame retardant according to claim 1, wherein the impurities in the step 2) comprise SiO2And unreacted C.
5. The method for preparing magnesium hydroxide as a flame retardant according to claim 1, wherein H is added in the step 3)2O2The pH of the solution is then 8-9.
6. The method for preparing magnesium hydroxide as a flame retardant of claim 1, wherein PEG is added to the solution filtered in the step 4) in addition to ammonia water.
7. The use of the flame retardant magnesium hydroxide prepared by the method of any one of claims 1 to 6 in ultra-high engineering plastic composites.
8. The use of claim 7, wherein the flame retardant magnesium hydroxide is made into a filter with ultra high molecular weight polyethylene by a sintering process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110941370.5A CN113620323A (en) | 2021-08-17 | 2021-08-17 | A kind of preparation method of flame retardant magnesium hydroxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110941370.5A CN113620323A (en) | 2021-08-17 | 2021-08-17 | A kind of preparation method of flame retardant magnesium hydroxide |
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| CN113620323A true CN113620323A (en) | 2021-11-09 |
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| CN202110941370.5A Pending CN113620323A (en) | 2021-08-17 | 2021-08-17 | A kind of preparation method of flame retardant magnesium hydroxide |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104743585A (en) * | 2015-03-04 | 2015-07-01 | 上海应用技术学院 | Method for preparing flame retardant grade magnesium hydroxide |
| CN105540622A (en) * | 2015-12-31 | 2016-05-04 | 上海应用技术学院 | Recycling and re-preparation method of silicon-steel level magnesium oxide |
| CN105984890A (en) * | 2015-02-26 | 2016-10-05 | 宝山钢铁股份有限公司 | Method for producing flame retardant grade magnesium hydrate from oriented silicon steel magnesium oxide waste |
| CN110002478A (en) * | 2018-01-05 | 2019-07-12 | 上海实业振泰化工有限公司 | The device and method of flake magnesium hydroxide and spherical magnesia is prepared with rear magnesia |
-
2021
- 2021-08-17 CN CN202110941370.5A patent/CN113620323A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984890A (en) * | 2015-02-26 | 2016-10-05 | 宝山钢铁股份有限公司 | Method for producing flame retardant grade magnesium hydrate from oriented silicon steel magnesium oxide waste |
| CN104743585A (en) * | 2015-03-04 | 2015-07-01 | 上海应用技术学院 | Method for preparing flame retardant grade magnesium hydroxide |
| CN105540622A (en) * | 2015-12-31 | 2016-05-04 | 上海应用技术学院 | Recycling and re-preparation method of silicon-steel level magnesium oxide |
| CN110002478A (en) * | 2018-01-05 | 2019-07-12 | 上海实业振泰化工有限公司 | The device and method of flake magnesium hydroxide and spherical magnesia is prepared with rear magnesia |
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Application publication date: 20211109 |
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