CN116216751A - Preparation process of magnesium hydroxide - Google Patents
Preparation process of magnesium hydroxide Download PDFInfo
- Publication number
- CN116216751A CN116216751A CN202310380668.2A CN202310380668A CN116216751A CN 116216751 A CN116216751 A CN 116216751A CN 202310380668 A CN202310380668 A CN 202310380668A CN 116216751 A CN116216751 A CN 116216751A
- Authority
- CN
- China
- Prior art keywords
- magnesium hydroxide
- temperature
- superfine
- rotary drum
- steam
- 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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Links
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 45
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 45
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 18
- 230000000694 effects Effects 0.000 claims abstract description 14
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000010902 jet-milling Methods 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 8
- 239000002861 polymer material Substances 0.000 abstract description 8
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- 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 description 6
- 239000003063 flame retardant Substances 0.000 description 6
- 229920000620 organic polymer Polymers 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention takes high-temperature calcined magnesia as a raw material, adopts a steam jet milling process, and after superfine treatment, the magnesia reacts with high-temperature steam in the superfine treatment process to hydrolyze to obtain magnesium hydroxide, and the magnesium hydroxide has low surface activity and good compatibility with high polymer materials, and can replace hexagonal flaky magnesium hydroxide products. The preparation technical process route of the invention comprises the following steps: (1) Crushing the high-temperature calcined magnesia by adopting steam airflow; (3) Hydrolyzing in a rotary drum to form magnesium hydroxide superfine powder; (4) bag dedusting and separating to obtain a magnesium hydroxide product. The invention is a new angle for preparing high-performance magnesium hydroxide products.
Description
Technical Field
The invention relates to a preparation process of magnesium hydroxide, and belongs to the technical field of fine chemical preparation.
Technical Field
The inorganic flame-retardant material is environment-friendly and low in cost, and is a trend of development of flame-retardant materials. The classical environment-friendly inorganic powder materials generally comprise magnesium hydroxide, aluminum hydroxide and magnesium aluminum hydrotalcite.
Magnesium hydroxide has alkalinity and can have a certain adverse effect on the weather resistance of an organic polymer material when being compounded with the organic polymer material. The magnesium hydroxide includes common magnesium hydroxide and hexagonal flaky magnesium hydroxide. The common magnesium hydroxide is cheap, has an amorphous structure, high surface or performance, large specific surface area and poor compatibility with organic polymer materials, and is applied to the field of low-end flame-retardant products; the hexagonal flaky magnesium hydroxide is ordered and crystalline, has uniform particle size distribution, good dispersion, low surface activity and good compatibility with organic polymer materials, is used in the field of high-end flame-retardant products, and has relatively high product price.
The preparation of hexagonal flaky magnesium hydroxide generally adopts precipitated magnesium hydroxide with higher activity as a raw material, and adopts hydrothermal treatment in an alkaline environment of sodium hydroxide solution, so that higher reaction temperature and reaction pressure are required, and after the reaction, the preparation method needs filter pressing washing, drying, concentrating and recovering filtrate, and has complex process and preparation cost.
The hexagonal flaky magnesium hydroxide has good application performance in the flame-retardant field, and the main reason is that the hexagonal flaky magnesium hydroxide is orderly arranged crystals, has smooth surface, low activity, uniform particle size distribution, good dispersion and good compatibility with organic polymer materials. The magnesium oxide calcined at high temperature has low activity, and magnesium hydroxide formed after hydrolysis has low activity, and compared with hexagonal flaky magnesium hydroxide prepared by a hydrothermal method, the magnesium hydroxide has better compatibility with organic polymers, and is more suitable for the use in the flame-retardant field. The magnesium oxide calcined at high temperature has low activity, and generally has slow reaction speed with water, so that the magnesium oxide is difficult to hydrolyze thoroughly.
The invention solves the technical problems existing in the classical preparation process, adopts high-temperature calcined magnesia as a raw material to prepare the superfine magnesium hydroxide powder material, and replaces hexagonal flaky magnesium hydroxide products.
Disclosure of Invention
The invention takes high-temperature calcined magnesia as a raw material, adopts a steam jet milling process, and after superfine treatment, the magnesia reacts with high-temperature steam and is hydrolyzed to obtain magnesium hydroxide in the superfine treatment process:
the invention comprises the following steps:
1. step one, taking high-temperature calcined magnesia as a raw material, and entering a steam jet milling equipment system for superfine treatment. The citric acid activity value of the high temperature calcined magnesia is in the range of 100 seconds to 1000 seconds, preferably 200 seconds to 600 seconds; the temperature of the steam flow for crushing is 180-280 ℃; the powder granularity of the air flow crushing system is required to have Dn90 smaller than 2 microns;
2. step two: the superfine magnesium oxide enters a rotary drum to react with high-temperature superheated steam in the drum to carry out high-temperature hydrolysis treatment, thus obtaining superfine magnesium hydroxide powder. The residence time of the powder in the rotary drum is from 2 to 12 hours, preferably from 4 to 6 hours; the superheated steam temperature in the rotary drum is 120 to 280 ℃, preferably 160 to 200 ℃.
3. Step three: and (5) feeding the magnesium hydroxide powder coming out of the rotary cylinder into a storage bin to obtain a magnesium hydroxide product.
The principle of the invention is as follows:
1. the magnesium oxide is calcined at a high temperature with low activity, and the magnesium hydroxide formed after hydrolysis has low activity, can have good compatibility with high polymer materials, and has better application performance in the flame-retardant field.
2. The method integrates steam jet milling and high-temperature steam hydrolysis, so that the magnesium oxide hydrolysis speed is increased, the magnesium oxide is thoroughly hydrolyzed, and the magnesium hydroxide powder material with high conversion rate is obtained.
Compared with the existing similar hexagonal flaky magnesium hydroxide products, the method has the beneficial effects that:
1. the invention integrates the superfine treatment and the hydrolysis, omits the process operations of hydrolysis, filtration, drying and the like in the reaction tank, has short preparation process, low energy consumption and low preparation cost.
2. The activity of the magnesium hydroxide product is lower than that of a hexagonal flaky magnesium hydroxide product, and the magnesium hydroxide product has wider prospect in the application field of high polymer materials.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention, in order to facilitate the understanding of those skilled in the art.
1. Adding the high-temperature calcined magnesia powder into a steam jet mill unit for superfine treatment. The particle size distribution of the high-temperature calcined magnesia is 80 to 400 meshes; citric acid activity to 300 seconds; the output of the steam jet mill unit is 0.5 ton/hour; the steam pressure used was 0.6MPa, the temperature 240℃and the steam flow rate was 2.5 tons/hour; the powder granularity Dn90 of the steam jet mill unit is smaller than 1.5 microns;
2. the superfine powder from the steam jet mill enters a rotary drum, reacts with part of high-temperature steam from the steam jet mill in the rotary drum, and hydrolyzes to form magnesium hydroxide. Maintaining the steam temperature in the rotary drum at 200 ℃ to 240 ℃; the residence time of the powder in the rotary drum is 6 hours;
3. and (5) feeding the magnesium hydroxide powder from the rotary cylinder into a storage bin, and packaging to obtain a magnesium hydroxide product.
Claims (3)
1. The preparation process of the magnesium hydroxide is characterized by comprising the following steps of:
step one, taking high-temperature calcined magnesia as a raw material, and entering a steam jet milling equipment system for superfine treatment;
secondly, enabling the superfine magnesium oxide to enter a rotary drum, reacting with high-temperature superheated steam in the rotary drum, and performing high-temperature hydrolysis treatment to obtain superfine magnesium hydroxide powder;
and thirdly, feeding the magnesium hydroxide powder from the rotary cylinder into a storage bin to obtain a magnesium hydroxide product.
2. The process for preparing magnesium hydroxide according to claim 1, wherein: taking high-temperature calcined magnesia as a raw material, and entering steam jet milling equipment to perform superfine treatment; the citric acid activity value of the high temperature calcined magnesia is in the range of 100 seconds to 1000 seconds, preferably 200 seconds to 600 seconds; the temperature of the steam flow for crushing is 180-280 ℃; the powder particle size of the air flow crushing device requires Dn90 to be less than 2 microns.
3. The process for preparing magnesium hydroxide according to claim 1, wherein: allowing the superfine magnesium oxide to enter a rotary drum, reacting with high-temperature superheated steam in the rotary drum, and performing high-temperature hydrolysis treatment to obtain superfine magnesium hydroxide powder, wherein the residence time of the powder in the rotary drum is 2-12 hours, preferably 4-6 hours; the superheated steam temperature in the rotary drum is 120 to 280 ℃, preferably 160 to 200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310380668.2A CN116216751A (en) | 2023-04-11 | 2023-04-11 | Preparation process of magnesium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310380668.2A CN116216751A (en) | 2023-04-11 | 2023-04-11 | Preparation process of magnesium hydroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116216751A true CN116216751A (en) | 2023-06-06 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310380668.2A Pending CN116216751A (en) | 2023-04-11 | 2023-04-11 | Preparation process of magnesium hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116216751A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774862A (en) * | 2012-08-14 | 2012-11-14 | 河北联合大学 | Method for preparing flame-retardant magnesium hydroxide by hydration |
| KR102112572B1 (en) * | 2019-10-01 | 2020-05-19 | 한국지질자원연구원 | Preparation of magnesium hydroxide powder from magnesite ore, and magnesium hydroxide powder obtained therefrom |
| CN112408440A (en) * | 2020-12-07 | 2021-02-26 | 上海实业振泰化工有限公司 | Process for preparing superfine coral velvet-shaped environment-friendly magnesium hydroxide by batch hydrothermal method |
| CN113353959A (en) * | 2021-06-22 | 2021-09-07 | 兰州交通大学 | Method for preparing magnesium hydroxide and calcium hydroxide flame retardant by using dolomite |
| CN114410128A (en) * | 2022-01-29 | 2022-04-29 | 辽宁鑫阳新材料科技有限公司 | Magnesium hydroxide ultra-fining and surface modification method and application thereof |
-
2023
- 2023-04-11 CN CN202310380668.2A patent/CN116216751A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774862A (en) * | 2012-08-14 | 2012-11-14 | 河北联合大学 | Method for preparing flame-retardant magnesium hydroxide by hydration |
| KR102112572B1 (en) * | 2019-10-01 | 2020-05-19 | 한국지질자원연구원 | Preparation of magnesium hydroxide powder from magnesite ore, and magnesium hydroxide powder obtained therefrom |
| CN112408440A (en) * | 2020-12-07 | 2021-02-26 | 上海实业振泰化工有限公司 | Process for preparing superfine coral velvet-shaped environment-friendly magnesium hydroxide by batch hydrothermal method |
| CN113353959A (en) * | 2021-06-22 | 2021-09-07 | 兰州交通大学 | Method for preparing magnesium hydroxide and calcium hydroxide flame retardant by using dolomite |
| CN114410128A (en) * | 2022-01-29 | 2022-04-29 | 辽宁鑫阳新材料科技有限公司 | Magnesium hydroxide ultra-fining and surface modification method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 丁志平: "《精细化工概论》", 31 August 2005, 化学工业出版社, pages: 9 * |
| 许珂敬: "《粉体工程学》", 中国石油大学出版社, pages: 133 * |
| 霍然等: "《建筑火灾安全工程导论》", 30 September 2009, 中国科学技术大学出版社, pages: 157 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zeng Weixing Inventor after: Xiao Yuanchun Inventor after: Lu Yahui Inventor before: Zeng Weixing Inventor before: Zeng Lian Inventor before: Xiao Yuanchun |
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| CB03 | Change of inventor or designer information |