CN1740269A - Liquid amonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant - Google Patents
Liquid amonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant Download PDFInfo
- Publication number
- CN1740269A CN1740269A CN 200510086473 CN200510086473A CN1740269A CN 1740269 A CN1740269 A CN 1740269A CN 200510086473 CN200510086473 CN 200510086473 CN 200510086473 A CN200510086473 A CN 200510086473A CN 1740269 A CN1740269 A CN 1740269A
- Authority
- CN
- China
- Prior art keywords
- ammonia
- magnesium hydroxide
- reactor
- precipitation
- hydrothermal
- 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.)
- Granted
Links
Images
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Fireproofing Substances (AREA)
Abstract
The present invention belongs to the field of inorganic chemical technology, and proposes one kind of liquid ammonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant. Through the first precipitation reaction of magnesium chloride material with liquid ammonia as precipitant at 15-90 deg.c and sealed and pressurized conditions to synthesize magnesium hydroxide, and the subsequent modification of the normal temperature synthesized magnesium hydroxide at 100-250 deg.c in the presence of dispersant of 0.01-0.1 % for 1-6 hr, magnesium hydroxide fire retardant is prepared, which has primary granularity of 0.3-2.0 micron, average coagulation particle size of 1.0-4.0 micron, specific surface area of 5-30 sq m/g, and magnesium hydroxide content over 98 %. The magnesium hydroxide fire retardant may be used in rubber, plastic, building material, etc.
Description
Technical field
This patent relates to a kind of novel process for preparing flame retardant of magnesium hydroxide, belongs to the inorganic chemical technology technical field.
Background technology
China is sea lake salt resource big country, mainly is distributed in province and coastland (as Tianjin, Dalian, Shandong etc.) such as Qinghai, Inner Mongol, Xinjiang, Tibet, Shanxi.Magnesium is the resource that reserves are only second to sodium in the sea lake salt.For a long time, be subjected to the restriction of technology and economic condition, the utilization of sea lake salt resource mainly concentrates on salt manufacturing or carries potassium, payes attention to not enough to the comprehensive utilization of by-product magnesium salts.Only there is few part magnesium salts to be used to produce magnesium chloride hexahydrate (100~300 yuan/ton) and magnesium sulfate heptahydrate primary products such as (500~600 yuan/ton) at present, be mainly used in building materials and metallurgy industry, the a large amount of high-magnesium brines that produce in the production process (content of magnesium chloride is up to 10~35% (w/v)) are in idle state mostly, form " magnesium evil ".Therefore, the outlet of magnesium salts is a problem that urgency is to be solved.
Along with the development of macromolecular materials such as plastics, rubber, synthon, its inflammableness also causes concern day by day.Especially when macromolecular material and electrical equipment are used in combination (as plastics such as electric wires), owing to work under conditions such as high pressure, heating, discharge, initiation fire easily burns.People work out anti-combustion and but the cigarette problem that various fire retardants solve macromolecular material for this reason.Compare with other fire retardant (as halogen system (chlorine system, bromine system), phosphorus system and inorganic combustion inhibitor (aluminium hydroxide, antimonous oxide etc.)), magnesium hydroxide has flame-retardant smoke inhibition, thermostability height (340~490 ℃ of decomposition temperatures), characteristics such as nontoxic, especially is fit to be used with thermally stable polymers such as PP, PA, POM.Therefore, demand high-purity, high-dispersion magnesium hydroxide combustion inhibitor enlarges just day by day, and its research and development are just becoming the focus of attention both domestic and external.
Israel Dead Sea bromine group is a raw material with high density chlorination magnesium bittern, adopt Pintsch process-hydrating process to prepare flame retardant of magnesium hydroxide, built up and produced ten thousand tons factory per year, this product purity height (>98%), pattern rule, good dispersity, China's wires and cables industry adopts the said firm's product mostly, import price up to 18,000 yuan/ton about; The characteristics of this technology are can be continuously, scale operation, and weak point is that facility investment is big, process energy consumption height, and a large amount of hydrochloric acid (170,000 tons of hydrochloric acid of 10,000 tons of magnesium hydroxide by-products) of by-product also need find new outlets (http: ∥ www.ameribrom.com) simultaneously.Ube company also builds up (the http: ∥ www.ubesh.com) of factory that utilizes seawater to produce flame retardant of magnesium hydroxide in dropping into huge fund in recent years.China only has several small-scale production factory at present, the annual output total amount of magnesium hydroxide is less than 20,000 tons, and size-grade distribution is wide mostly, purity is low, and (magnesium hydroxide content is lower than 96% mostly, minority can reach more than 98% with ammoniacal liquor synthetic product purity), reunite serious, make its price cheap (generally being lower than 7000 yuan/ton), application surface is limited; And added value is higher, the market requirement increases faster that high-purity high-dispersion magnesium hydroxide fire retardant output is very little, cause the required high-performance flame retardant of magnesium hydroxide overwhelming majority dependence on import of industries such as China's plastics, rubber, electric wire, form a sharp contrast with a large amount of idle magnesium resource present situations.
Domestic many units are to synthetic research, employing ammoniacal liquor (Sun Qingguo, Xiao Xueying, Song Mingli, Meng Ruiying, the preparation of high-dispersion magnesium hydroxide, salt lake research, 1999,7 (2), the 35-42 of having carried out of magnesium hydroxide.), sodium hydroxide (Li Zhiqiang, Wu Qingliu, to orchid, Wei Fei, the influence that the normal temperature synthesis condition prepares the flame retardant of magnesium hydroxide pilot scale research to two-step approach, chemical industry journal, 2005,56 (6), 1106-1111; Sun Yongming, money petrel, Liu Jianlan, Yu Bin, dispersion agent is to the experimental study of preparation super fine magnesium hydroxide influence, nonmetalliferous ore, 2005,28 (4), 54-56), calcium hydroxide (Liu Yusheng, Liu Cui, Ma Peihua utilizes salt lake brine to produce the technology exploration of magnesium hydroxide, salt lake research, 2004,12 (2), 51-55.), microgravity (Song Yunhua, Chen Jianming, Liu Lihua, Guo Fen, high-gravity technology prepare the applied research of nano-magnesium hydrate fire retardant, chemical industry mineral and processing, 2004,5,19-23.) etc. method prepare flame retardant of magnesium hydroxide.The ammoniacal liquor method generally adopts industrial ammonia to carry out in non-pressure vessel, the product purity that makes is higher, shortcoming is ammonia concn low (<30%), a high volatility under the condition of normal pressure, a large amount of low concentration ammonium chlorides that process produces are difficult to recycling, and the utilization ratio of ammonia is low, wastewater flow rate big, work under bad environment; The product purity height that sodium hydroxide method makes, pattern rule, but raw materials cost is higher and product solid-liquid separation difficulty; Calcium hydroxide method technology is simple, with low cost, but generally contains more calcium impurities in the product, is difficult to make high purity product; The particle that the microgravity method generates is tiny, but the solid-liquid separation difficulty, reunite serious and the process energy consumption bigger.In addition, because magnesium hydroxide is the very strong compound of a kind of surface polarity, so ordinary method synthetic product often is easy to reunite, dispersiveness and consistency are all relatively poor when directly adding in the superpolymer, influence the processing characteristics of matrix material, need that it is carried out modification and handle (Li Zhiqiang, Wu Qingliu, to orchid, Wei Fei, the hydrothermal modification condition is to the influence of preparation flame retardant of magnesium hydroxide pilot scale research, the chemical industry journal, 2005,56 (7), 1349-1354; Li Zhiqiang, Wu Qingliu, to orchid, Wei Fei, the temperature research that preparation influences to flame retardant of magnesium hydroxide, sea lake salt and chemical industry, 2004,33 (5), 1-4).
Summary of the invention
In order to overcome low, the shortcomings such as wastewater flow rate big, work under bad environment of utilization ratio of the ammonia that present ammoniacal liquor method exists, the present invention proposes to adopt liquefied ammonia pressurized precipitation-hydrothermal modification novel process to prepare flame retardant of magnesium hydroxide.Not only technology is simple, easy to operate, with low cost for this method, non-environmental-pollution, and product purity height, pattern rule, favorable dispersity.
Technical scheme of the present invention is as follows:
A kind of liquefied ammonia pressurized precipitation-hydrothermal modification legal system is equipped with the method for flame retardant of magnesium hydroxide, it is characterized in that: this method is raw material with the magnesium chloride, and liquefied ammonia is precipitation agent, carries out liquid-phase precipitation and hydrothermal modification and handle in airtight pressurized reactor, the preparation flame retardant of magnesium hydroxide, concrete steps are as follows:
1) be that the magnesium chloride solution of 10~40% (w/v) adds closed reactor with concentration, the speed with 0.7~2.8 mole/minute under 15~90 ℃ and stirring state feeds liquefied ammonia, and wherein the mol ratio of magnesium salts and liquefied ammonia is 1: 1~2; After logical ammonia finished, blasting air, to keep reactor pressure be 0.05~0.5MPa, continues reaction 0.5~3 hour, and the gas that will contain air and unreacted ammonia after reaction finishes enters ammonia recovery unit;
2) reaction product in the above-mentioned reactor is filtered, washed; Under agitation condition, filter cake made concentration and is 5~30% slurries;
3) above-mentioned slurries are added hydrothermal reactor, and then add dispersion agent in hydrothermal reactor, its weight is 0.01~0.1% of described slurry weight, stirs 1~6 hour at 100~250 ℃ of constant temperature; Wherein, dispersion agent is polyacrylic acid, Sodium hexametaphosphate 99, ethanol or Sodium dodecylbenzene sulfonate;
4) be 0.3~2.0 μ m with obtaining the primary particle diameter of particle after the cooling of the slurry after the hydrothermal treatment consists, filtration, washing, drying, the pulverizing, aggregated particle size 1.0~4.0 μ m, specific surface area 5~30m
2/ g, purity is greater than 98% pattern rule, the magnesium hydroxide sheet product of favorable dispersity;
5) adopt unslaked lime method recycling step 2) ammonia in the filtrate, the ammonia of overflowing is entered ammonia recovery unit;
6) in ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
The characteristics of technology of the present invention are: (1) industrial liquefied ammonia based on very high purity (>98.5%), help preparing high purity product, and it is directly fed the ammonia concentration that can improve reaction system in the high density chlorination magnesium solution, reduce the process water consumption; (2) adopt the pressurized fluid ammonia precipitation both can improve solubleness, utilization ratio and the speed of response of ammonia in water, also can avoid ammonia to overflow, avoid environmental pollution; (3) adopt dispersion agent and hydrothermal modification technology further to improve the pattern and the dispersiveness of magnesium hydroxide; (4) ammonium chloride in the normal temperature synthetic filtrate and the equal reusable edible of unreacted ammonia had not only reduced cost but also non-environmental-pollution.
Similar work does not appear in the newspapers both at home and abroad as yet.The comprehensive cost that adopts the high-performance flame retardant of magnesium hydroxide of this prepared is 3000-4000 unit/ton, and the present price of analogous products is 18,000 yuan/ton, and economic benefit is very remarkable.The flame retardant of magnesium hydroxide of the present invention's preparation can be used for industries such as rubber, plastics, electric wire and building materials and prepares the high-performance composite flame-proof material, has a extensive future.
Description of drawings
Fig. 1 changes the process flow diagram that legal system is equipped with flame retardant of magnesium hydroxide for liquefied ammonia pressurized precipitation-hydro-thermal.
Fig. 2 is the microscopic appearance of magnesium hydroxide normal temperature product.
Fig. 3 is the microscopic appearance of magnesium hydroxide hydrothermal product.
Fig. 4 is the X-ray powder diffraction pattern of magnesium hydroxide hydrothermal product.
Embodiment
Liquefied ammonia pressurized precipitation-hydrothermal modification legal system that the present invention proposes is equipped with the method for flame retardant of magnesium hydroxide, as shown in Figure 1, is raw material with the magnesium chloride, liquefied ammonia is precipitation agent, in airtight pressurized reactor, carry out liquid-phase precipitation and hydrothermal modification and handle, the preparation flame retardant of magnesium hydroxide, concrete steps are as follows:
1) be that the magnesium chloride solution of 10~40% (w/v) adds closed reactor with concentration, the speed with 0.7~2.8 mole/minute under 15~90 ℃ and stirring state feeds liquefied ammonia, and wherein the mol ratio of magnesium salts and liquefied ammonia is 1: 1~2; After logical ammonia finished, blasting air, to keep reactor pressure be 0.05~0.5MPa, continues reaction 0.5~3 hour, and the gas that will contain air and unreacted ammonia after reaction finishes enters ammonia recovery unit;
2) reaction product in the above-mentioned reactor is filtered, washed; Under agitation condition, filter cake made concentration and is 5~30% slurries;
3) above-mentioned slurries are added hydrothermal reactor, and then add dispersion agent in hydrothermal reactor, its weight is 0.01~0.1% of described slurry weight, stirs 1~6 hour at 100~250 ℃ of constant temperature; Wherein, dispersion agent is polyacrylic acid, Sodium hexametaphosphate 99, ethanol or Sodium dodecylbenzene sulfonate;
4) be 0.3~2.0 μ m with obtaining the primary particle diameter of particle after the cooling of the slurry after the hydrothermal treatment consists, filtration, washing, drying, the pulverizing, aggregated particle size 1.0~4.0 μ m, specific surface area 5~30m
2/ g, purity is greater than 98% pattern rule, the magnesium hydroxide sheet product of favorable dispersity;
5) adopt unslaked lime method recycling step 2) ammonia in the filtrate, the ammonia of overflowing is entered ammonia recovery unit;
6) in ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Describe content of the present invention in detail below in conjunction with specific embodiment.
Embodiment 1
Prepare 40 liter of 10% (w/v) magnesium chloride solution and add closed reactor, at 15 ℃, stir under (150 rev/mins) condition and at the uniform velocity fed (0.7 mole/minute) liquefied ammonia 1 hour, blasting air after logical ammonia finishes, to keep reactor pressure be 0.05MPa, continues reaction 3 hours.Reaction enters ammonia recovery unit with gas phase after finishing, after slurry filtration, the washing, be 5% slurries and add hydrothermal reactor stirring to make under (150 rev/mins) condition to contain admittedly, add 0.1% polyacrylic acid then, stir (150 rev/mins) reaction 6 hours at 250 ℃ of constant temperature, cool off then, filter, wash, obtain the average primary particle diameter 2.0 μ m of particle after the drying (105 ℃, 4 hours), pulverizing, average aggregated particle size 3.0 μ m, specific surface area 5m
2/ g, the hexagonal flake magnesium hydroxide particle of purity 99.5%.Normal temperature synthetic filtrate and 5.2 kilograms of unslaked limes are put into airtight ammonia still process container, be heated to 100-105 ℃, the ammonia of overflowing is entered retrieving arrangement.In ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Embodiment 2
Prepare 40 liter of 40% (w/v) magnesium chloride solution and add closed reactor, at 90 ℃, stir under (150 rev/mins) condition and at the uniform velocity fed (2.8 moles/minute) liquefied ammonia 1 hour, blasting air after logical ammonia finishes, to keep reactor pressure be 0.5MPa, continues reaction 1 hour.Reaction enters ammonia recovery unit with gas phase after finishing, after slurry filtration, the washing, be 30% slurries and add hydrothermal reactor stirring to make under (150 rev/mins) condition to contain admittedly, add 0.01% Sodium hexametaphosphate 99 then, stir (150 rev/mins) reaction 1 hour at 100 ℃ of constant temperature, cool off then, filter, wash, obtain the average primary particle diameter 0.5 μ m of particle after the drying (105 ℃, 4 hours), pulverizing, average aggregated particle size 4.0 μ m, specific surface area 30m
2/ g, the hexagonal flake magnesium hydroxide particle of purity 98.0%.Normal temperature synthetic filtrate and 21.5 kilograms of unslaked limes are put into airtight ammonia still process container, be heated to 100-105 ℃, the ammonia of overflowing is entered retrieving arrangement.In ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Embodiment 3
Prepare 40 liter of 20% (w/v) magnesium chloride solution and add closed reactor, at 40 ℃, stir under (150 rev/mins) condition and at the uniform velocity fed (1.5 moles/minute) liquefied ammonia 1 hour, blasting air after logical ammonia finishes, to keep reactor pressure be 0.2MPa, continues reaction 3 hours.Reaction enters ammonia recovery unit with gas phase after finishing, after slurry filtration, the washing, be 15% slurries and add hydrothermal reactor stirring to make under (150 rev/mins) condition to contain admittedly, add 0.05% ethanol then, stir (150 rev/mins) reaction 4 hours at 180 ℃ of constant temperature, cool off then, filter, wash, obtain the average primary particle diameter 1.0 μ m of particle after the drying (105 ℃, 4 hours), pulverizing, average aggregated particle size 2.0 μ m, specific surface area 15m
2/ g, the hexagonal flake magnesium hydroxide particle of purity 98.5%.Normal temperature synthetic filtrate and 10.8 kilograms of unslaked limes are put into airtight ammonia still process container, be heated to 100-105 ℃, the ammonia of overflowing is entered retrieving arrangement.In ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Embodiment 4
Prepare 40 liter of 20% (w/v) magnesium chloride solution and add closed reactor, at 60 ℃, stir under (150 rev/mins) condition and at the uniform velocity fed (1.5 moles/minute) liquefied ammonia 1 hour, blasting air after logical ammonia finishes, to keep reactor pressure be 0.05MPa, continues reaction 2 hours.Reaction enters ammonia recovery unit with gas phase after finishing, after slurry filtration, the washing, be 5% slurries and add hydrothermal reactor stirring to make under (150 rev/mins) condition to contain admittedly, add 0.05% Sodium dodecylbenzene sulfonate then, stir (150 rev/mins) reaction 4 hours at 220 ℃ of constant temperature, cool off then, filter, wash, obtain the average primary particle diameter 1.2 μ m of particle after the drying (105 ℃, 4 hours), pulverizing, average aggregated particle size 1.5 μ m, specific surface area 20m
2/ g, the hexagonal flake magnesium hydroxide particle of purity 99.2%.Normal temperature synthetic filtrate and 10.8 kilograms of unslaked limes are put into airtight ammonia still process container, be heated to 100-105 ℃, the ammonia of overflowing is entered retrieving arrangement.In ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Embodiment 5
Prepare 40 liter of 20% (w/v) magnesium chloride solution and add closed reactor, at 40 ℃, stir under (150 rev/mins) condition and at the uniform velocity fed (1.5 moles/minute) liquefied ammonia 1 hour, blasting air after logical ammonia finishes, to keep reactor pressure be 0.3MPa, continues reaction 3 hours.Reaction enters ammonia recovery unit with gas phase after finishing, after slurry filtration, the washing, be 15% slurries and add hydrothermal reactor stirring to make under (150 rev/mins) condition to contain admittedly, add 0.1% Sodium dodecylbenzene sulfonate then, stir (150 rev/mins) reaction 6 hours at 200 ℃ of constant temperature, cool off then, filter, wash, obtain the average primary particle diameter 0.8 μ m of particle after the drying (105 ℃, 4 hours), pulverizing, average aggregated particle size 1.5 μ m, specific surface area 10m
2/ g, the hexagonal flake magnesium hydroxide particle of purity 99%.Normal temperature synthetic filtrate and 10.8 kilograms of unslaked limes are put into airtight ammonia still process container, be heated to 100-105 ℃, the ammonia of overflowing is entered retrieving arrangement.In ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.Fig. 2 represents the scanning electron microscope pattern of embodiment 5 gained normal temperature products, and Fig. 3 represents the scanning electron microscope pattern of embodiment 5 gained hydrothermal products, and Fig. 4 represents the X-ray powder diffraction spectrogram of embodiment 5 gained hydrothermal products.The above results shows, adopts the present invention can make the high purity magnesium hydroxide fire retardant of pattern rule, uniform particle diameter, favorable dispersity.
Embodiment 6
Prepare 40 liter of 40% (w/v) magnesium chloride solution and add closed reactor, at 40 ℃, stir under (150 rev/mins) condition and at the uniform velocity fed (2.8 moles/minute) liquefied ammonia 1 hour, blasting air after logical ammonia finishes, to keep reactor pressure be 0.1MPa, continues reaction 3 hours.Reaction enters ammonia recovery unit with gas phase after finishing, after slurry filtration, the washing, be 10% slurries and add hydrothermal reactor stirring to make under (150 rev/mins) condition to contain admittedly, add 0.08% Sodium dodecylbenzene sulfonate then, stir (150 rev/mins) reaction 6 hours at 250 ℃ of constant temperature, cool off then, filter, wash, obtain the average primary particle diameter 0.3 μ m of particle after the drying (105 ℃, 4 hours), pulverizing, average aggregated particle size 1.0 μ m, specific surface area 15m
2/ g, the hexagonal flake magnesium hydroxide particle of purity 98.8%.Normal temperature synthetic filtrate and 21.5 kilograms of unslaked limes are put into airtight ammonia still process container, be heated to 100-105 ℃, the ammonia of overflowing is entered retrieving arrangement.In ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Claims (1)
1. liquefied ammonia pressurized precipitation-hydrothermal modification legal system is equipped with the method for flame retardant of magnesium hydroxide, it is characterized in that: this method is raw material with the magnesium chloride, and liquefied ammonia is precipitation agent, carries out liquid-phase precipitation and hydrothermal modification and handle in airtight pressurized reactor, the preparation flame retardant of magnesium hydroxide, concrete steps are as follows:
1) be that the magnesium chloride solution of 10~40%w/v adds closed reactor with concentration, the speed with 0.7~2.8 mole/minute under 15~90 ℃ and stirring state feeds liquefied ammonia, and wherein the mol ratio of magnesium salts and liquefied ammonia is 1: 1~2; After logical ammonia finished, blasting air, to keep reactor pressure be 0.05~0.5MPa, continues reaction 0.5~3 hour, and the gas that will contain air and unreacted ammonia after reaction finishes enters ammonia recovery unit;
2) reaction product in the above-mentioned reactor is filtered, washed; Under agitation condition, filter cake made concentration and is 5~30% slurries;
3) above-mentioned slurries are added hydrothermal reactor, and then add dispersion agent in hydrothermal reactor, its weight is 0.01~0.1% of described slurry weight, stirs 1~6 hour at 100~250 ℃ of constant temperature; Wherein, dispersion agent is polyacrylic acid, Sodium hexametaphosphate 99, ethanol or Sodium dodecylbenzene sulfonate;
4) be 0.3~2.0 μ m with obtaining the primary particle diameter of particle after the cooling of the slurry after the hydrothermal treatment consists, filtration, washing, drying, the pulverizing, aggregated particle size 1.0~4.0 μ m, specific surface area 5~30m
2/ g, purity is greater than 98% pattern rule, the magnesium hydroxide sheet product of favorable dispersity;
5) adopt unslaked lime method recycling step 2) ammonia in the filtrate, the ammonia of overflowing is entered ammonia recovery unit;
6) in ammonia recovery unit, ammonia is separated, pressurization, liquefaction, and recirculation is used for pressurized fluid ammonia precipitation operation.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2005100864739A CN100375778C (en) | 2005-09-23 | 2005-09-23 | Liquid amonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2005100864739A CN100375778C (en) | 2005-09-23 | 2005-09-23 | Liquid amonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1740269A true CN1740269A (en) | 2006-03-01 |
CN100375778C CN100375778C (en) | 2008-03-19 |
Family
ID=36092803
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2005100864739A Expired - Fee Related CN100375778C (en) | 2005-09-23 | 2005-09-23 | Liquid amonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100375778C (en) |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102211760A (en) * | 2010-03-26 | 2011-10-12 | 富士胶片株式会社 | Method for producing metal hydroxide fine particle |
CN104071813A (en) * | 2014-07-08 | 2014-10-01 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide |
US9061919B2 (en) | 2009-10-02 | 2015-06-23 | Tateho Chemical Industries Co., Ltd. | Magnesium oxide powder having excellent dispersibility and method for producing the same |
CN105926002A (en) * | 2016-05-20 | 2016-09-07 | 西北师范大学 | Method for preparing sheet-shaped nanometer Mg(OH)2 by using electrolyte diaphragm discharge plasma |
CN106082286A (en) * | 2016-06-06 | 2016-11-09 | 中南大学 | A kind of thermal battery electrolyte inhibitor MgO and preparation method thereof |
CN106365186A (en) * | 2016-09-29 | 2017-02-01 | 益盐堂(应城)健康盐制盐有限公司 | Method and device for achieving continuous production of magnesium hydrate with controllable particle size and span |
CN109162148A (en) * | 2018-09-20 | 2019-01-08 | 何治伟 | A kind of preparation method of primary composite modified fire retardant papers material |
CN111164048A (en) * | 2017-11-17 | 2020-05-15 | 株式会社Lg化学 | Method for recovering supercritical waste liquid generated in preparation process of silica aerogel felt |
CN113697831A (en) * | 2021-09-29 | 2021-11-26 | 安徽大学绿色产业创新研究院 | Method for purifying and removing magnesium from industrial wastewater with high sodium-magnesium ratio and preparing magnesium hydroxide fire retardant |
CN114890445A (en) * | 2022-06-08 | 2022-08-12 | 辽宁麦格尼科技有限公司 | Method for synthesizing superfine magnesium hydroxide by continuous liquid membrane |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AT392774B (en) * | 1989-05-05 | 1991-06-10 | Veitscher Magnesitwerke Ag | FINE POWDERED MAGNESIUM HYDROXIDE AND METHOD FOR THE PRODUCTION THEREOF |
IL112385A (en) * | 1994-01-21 | 1998-08-16 | Flamemag International Gie | Process for preparing a flame retardant magnesium hydroxide |
-
2005
- 2005-09-23 CN CNB2005100864739A patent/CN100375778C/en not_active Expired - Fee Related
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9061919B2 (en) | 2009-10-02 | 2015-06-23 | Tateho Chemical Industries Co., Ltd. | Magnesium oxide powder having excellent dispersibility and method for producing the same |
CN102211760A (en) * | 2010-03-26 | 2011-10-12 | 富士胶片株式会社 | Method for producing metal hydroxide fine particle |
CN104071813A (en) * | 2014-07-08 | 2014-10-01 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide |
CN105926002A (en) * | 2016-05-20 | 2016-09-07 | 西北师范大学 | Method for preparing sheet-shaped nanometer Mg(OH)2 by using electrolyte diaphragm discharge plasma |
CN106082286A (en) * | 2016-06-06 | 2016-11-09 | 中南大学 | A kind of thermal battery electrolyte inhibitor MgO and preparation method thereof |
CN106365186A (en) * | 2016-09-29 | 2017-02-01 | 益盐堂(应城)健康盐制盐有限公司 | Method and device for achieving continuous production of magnesium hydrate with controllable particle size and span |
JP2020529960A (en) * | 2017-11-17 | 2020-10-15 | エルジー・ケム・リミテッド | Regeneration method of supercritical waste liquid generated during the manufacturing process of silica airgel blanket |
CN111164048A (en) * | 2017-11-17 | 2020-05-15 | 株式会社Lg化学 | Method for recovering supercritical waste liquid generated in preparation process of silica aerogel felt |
JP7060675B2 (en) | 2017-11-17 | 2022-04-26 | エルジー・ケム・リミテッド | Regeneration method of supercritical waste liquid generated during the manufacturing process of silica airgel blanket |
CN111164048B (en) * | 2017-11-17 | 2023-04-28 | 株式会社Lg化学 | Method for recycling supercritical waste liquid generated in preparation process of silica aerogel felt |
US11760645B2 (en) | 2017-11-17 | 2023-09-19 | Lg Chem, Ltd. | Method for recycling supercritical waste liquid generated during process of producing silica aerogel blanket |
US11981576B2 (en) | 2017-11-17 | 2024-05-14 | Lg Chem, Ltd. | Method for recycling supercritical waste liquid generated during process of producing silica aerogel blanket |
CN109162148A (en) * | 2018-09-20 | 2019-01-08 | 何治伟 | A kind of preparation method of primary composite modified fire retardant papers material |
CN113697831A (en) * | 2021-09-29 | 2021-11-26 | 安徽大学绿色产业创新研究院 | Method for purifying and removing magnesium from industrial wastewater with high sodium-magnesium ratio and preparing magnesium hydroxide fire retardant |
CN114890445A (en) * | 2022-06-08 | 2022-08-12 | 辽宁麦格尼科技有限公司 | Method for synthesizing superfine magnesium hydroxide by continuous liquid membrane |
CN114890445B (en) * | 2022-06-08 | 2024-01-26 | 辽宁麦格尼科技有限公司 | Method for synthesizing superfine magnesium hydroxide by continuous liquid film |
Also Published As
Publication number | Publication date |
---|---|
CN100375778C (en) | 2008-03-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100375778C (en) | Liquid amonia pressurized precipitation and hydrothermal modification process for preparing magnesium hydroxide fire retardant | |
CN112876738B (en) | High-performance calcium sulfate whisker material and preparation process thereof | |
CN101559973B (en) | Method for preparing nano zinc oxide and crystal whisker zinc oxide by using industrial zinc sulfate as raw material | |
CN102531001B (en) | Comprehensive soda ash producing process and product application thereof | |
CN110642274B (en) | Method for preparing hexagonal flaky magnesium hydroxide for flame retardant by hydrothermal method of large-particle-size magnesium hydroxide | |
CN102502726B (en) | Preparation method for hexagonal sheet magnesium hydroxide | |
CN101717999A (en) | Method for preparing calcium sulfate whisker by crystal seed alcohol heating method | |
CN100386263C (en) | Water heat modification method for high dispersion magnesium hydroxide nanometer sheet | |
CN1830787A (en) | Method of preparing high purity magnesium oxide by closed pyrolysis magnesium chloride hydrate | |
CN102030348B (en) | Device and method for continuously preparing magnesium hydroxide flame retardant | |
CN1252295C (en) | Method of preparing high purity magnesiun sand using salt lake bischofite as raw material | |
CN111547750A (en) | Preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size | |
CN101177289A (en) | Method for preparing fibrous nano magnesium hydrate | |
CN110526272B (en) | Micro-nano structure CeCO3Preparation process of OH | |
Wang et al. | Preparation, properties and phase transition of mesoporous hydromagnesite with various morphologies from natural magnesite | |
CN101219801A (en) | Process for producing nano-flame-proof magnesium hydroxide | |
CN109437261A (en) | A kind of sheeted nanometer magnesium hydroxide raw powder's production technology | |
CN104609449A (en) | Method for preparing high dispersed magnesium hydroxide from agglomerated state magnesium hydroxide | |
CN102060314A (en) | Preparation method for synthesizing platy flame-retardant magnesium hydroxide by using light burned magnesia powder | |
CN109052446B (en) | Method for preparing calcium-aluminum hydrotalcite by using industrial waste residues as raw materials | |
CN115231593A (en) | Method for preparing hexagonal magnesium hydroxide flame retardant by one-step hydrothermal method | |
CN102703982A (en) | Method for preparing magnesium carbonate trihydrate crystal whisker by utilizing serpentine | |
CN1183037C (en) | Process for preparing magnesium hydroxide whisker | |
CN1401574A (en) | Process for preparing high dispersion flake magnesium hydroxide | |
CN102205971A (en) | Method for preparing ammonium illite sheets, alumina silicate sheets, and nano-sized kaolinite |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080319 Termination date: 20180923 |