CN1132784C - One-step process of producing magnesium hydroxide - Google Patents
One-step process of producing magnesium hydroxide Download PDFInfo
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- CN1132784C CN1132784C CN 01127343 CN01127343A CN1132784C CN 1132784 C CN1132784 C CN 1132784C CN 01127343 CN01127343 CN 01127343 CN 01127343 A CN01127343 A CN 01127343A CN 1132784 C CN1132784 C CN 1132784C
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- magnesium hydroxide
- magnesium
- produced
- ammoniacal liquor
- single stage
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Abstract
The present invention relates to a production method for compounds of metal magnesium, particularly to a magnesium hydroxide production method. Brine containing magnesium chloride is mixed with and ammonia water according to the proportion of 1:2.0 to 1:1.3 between magnesium chloride and free ammonia, and a reaction for 5 to 30 minutes at the temperature of 45 to 90 DEG C in the mixture; reaction liquid is filtered, washed, dried and pulverized to obtain magnesium hydroxide solid. The production of magnesium hydroxide by the one-step method thoroughly solves the problem of the scabbing of equipment pipelines existing in the production of magnesium hydroxide by a two-step method, intermittent operation is changed into continuous production, and constant operating conditions are used; Obtained products have the advantages of high quality and stability and can be used as high-quality flame retardants; the medicine level can be reached. The present invention has the advantages of operating condition reduction, low reaction temperature, energy consumption due to the use of residual heat discharged during the preparation of ammonia water, and fresh water resource saving in a large amount.
Description
Technical field
The present invention relates to the production method of the compound of MAGNESIUM METAL, especially the production method of magnesium hydroxide.
Background technology
Bittern is meant the occurring in nature saltiness greater than 3.5% the aqueous solution, and the bittern comprehensive utilization can obtain Chemicals such as salt, saltcake, Repone K, sal epsom, thenardite, bariumchloride, borax, boric acid, soda ash, bromine, iodine.Bittern can be divided into three kinds of main types according to its chemical composition: carbonate type, sulfate type and chloride type, no matter the bittern of the sort of type all contains abundant magnesium ion.
Fire retardant can be divided into organic fire-retardant and inorganic combustion inhibitor, and organic fire-retardant can produce a large amount of deleterious dense smokes and obnoxious flavour when burning.Along with science and technology development, people more and more pay attention to environment protection, and organic fire-retardant will be replaced by nontoxic inorganic combustion inhibitor.Magnesium hydroxide is the outstanding typical case of in inorganic combustion inhibitor family representative, its Heat stability is good, efficient, press down cigarette, nontoxic, environmentally safe.
Producing magnesium hydroxide can have several different methods, and for example more common seawater can generate magnesium hydroxide with the Wingdale reaction, but that traditional production method ubiquity long flow path, reaction conditions require is high, equipment installation defective such as scab seriously in the reaction process." brief talking the magnesium hydroxide production method " literary composition of publishing in " magnesium salts industry " magazine of the second phase in 2000 describes the process of producing magnesium hydroxide with bittern and ammonia two-step approach in detail: the first step is carried out the cold reaction under the low temperature, and second goes on foot High Temperature High Pressure thermal response again.This method is owing to comprise the High Temperature High Pressure thermal process reactor, and production cost height, production cycle length, equipment installation scab seriously.
Summary of the invention
In order to overcome the above-mentioned defective that traditional production method exists, the invention provides the method that a kind of flow process is short, reaction conditions is low, the single stage method of less investment is produced magnesium hydroxide.Its technical scheme is: will contain the bittern of magnesium chloride and ammoniacal liquor is 1 according to the mol ratio of magnesium chloride and free ammonia: the mixed of 1.3-2.0, and mixture was reacted 5-30 minute in 45 ℃-90 ℃ environment, will obtain solid hydrogen magnesium oxide after the filtration of reaction solution process, washing, drying, the pulverizing.
As to further improvement of the present invention, the reaction solution of bittern and ammoniacal liquor at first once can also be filtered, filtered liquid after once filtering prepares ammoniacal liquor through adding lime ammonia still process, filter cake after once filtering carries out secondary filtration after adding the water making beating again, the filter cake of secondary filtration makes solid hydrogen magnesium oxide again through super-dry, pulverizing.
As further improving of the present invention, its proportioning was that the mol ratio according to magnesium chloride and aqua ammonia is 1 when above-mentioned bittern reacted with ammoniacal liquor: the mixed of 1.3-1.65, and mixture is reacted in 50 ℃-60 ℃ environment.
The technical program can be under lower temperature, and primary first-order equation just can obtain magnesium hydroxide, has thoroughly solved the problem that pipeline scabs, and can continuous production, and operational condition is constant, good product quality and stable.Reduced operational condition, temperature of reaction is low, less investment.
Description of drawings
Accompanying drawing is the process flow sheet of one embodiment of the present of invention.
Embodiment
Embodiment 1:
As shown in drawings, at first prepare qualified hot ammoniacal liquor and purified bittern, measure wherein magnesium chloride and the content of free ammonia, according to the mol ratio of magnesium chloride and free ammonia is that 1: 1.6 mixed is sent in the reactor, at stirring reaction under 50 ℃ the temperature after 20 minutes, to react liquid pump to No. time filter and carry out solid-liquid separation and washing, the filtered liquid after once filtering prepares ammoniacal liquor through adding lime ammonia still process, and ammoniacal liquor can be used as the raw material of producing magnesium hydroxide again; Filter cake after once filtering carries out secondary filtration after adding the water making beating again, sends solid materials to the making beating still, adds after the fresh water making beating again that pump to secondary filtration machine filters and washs, and filter and secondary filtration machine can use common pressure filter.Solid materials behind the secondary filtration is delivered to drying in the flash dryer, promptly can be packed after the pulverizing in the fluidized bed type micronizer mill.
The filtrate of separating from a filter is contained more ammonium ion, can deliver to add lime in the mother vat, adopts the ammonia still process method to prepare ammoniacal liquor, and the ammoniacal liquor of producing can be used as raw material again and is used to produce magnesium hydroxide.
In order to improve the purity of product, once repeating the filtering process of repeatedly pulling an oar between filtration and the secondary filtration, till the purity of magnesium hydroxide meets the requirements.
The magnesium hydroxide products quality index that adopts present embodiment to obtain is as follows:
Magnesium hydroxide content＞99.5%
Product saliferous (in chlorion)＜0.1%
Product is moisture＜and 0.3%
Product contains SO
4 2-＜0.4%
Specific surface area＜15m
2/ g
Product cut size: 3 μ m are following by filtering greater than 95%
Embodiment 2: production stage is with embodiment 1, and the mol ratio of magnesium chloride and free ammonia is 1: 1.6, and stirring reaction is 30 minutes under 80 ℃ the temperature, obtains solid hydrogen magnesium oxide by filtration-making beating-filtration-exsiccant process then.
Embodiment 3: production stage is with embodiment 1, and the mol ratio of magnesium chloride and free ammonia is 1: 2, and stirring reaction is 10 minutes under 70 ℃ the temperature, obtains solid hydrogen magnesium oxide by filtration-making beating-filtration-exsiccant process then.
In technical scheme of the present invention, the proportioning of ammoniacal liquor and bittern should be that the consumption of ammoniacal liquor is The more the better, the consumption of ammoniacal liquor more at most magnesium hydroxide separate out thorough more, speed of response is fast more, but consider the factor of production cost aspect, the consumption of ammoniacal liquor should be not less than 1.3 times of theoretical consumption.When being lower than 1.3 times consumption, may have in the bittern that more magnesium ion is residual can not separate out, the reaction times also will prolong, and production cost is higher; When the consumption of ammoniacal liquor was higher than 2 times of theoretical consumption, the ammoniacal liquor waste was more, and production cost is higher equally, preferably technical scheme be the consumption of ammoniacal liquor be theoretical consumption 1.3-1.6 doubly, the best techniques scheme is that the consumption of ammoniacal liquor is 1.6 times of theoretical consumption.
Reaction times in reactor will be determined according to the temperature in when reaction and the concentration of ammoniacal liquor.Because temperature of reaction is lower, the time is shorter, therefore can carry out in the tank reactor continuously, realizes continuous production.
Single stage method is produced magnesium hydroxide and has thoroughly been solved a difficult problem-equipment installation that exists during two-step approach the is produced problem that scabs, the change intermittent operation is continuous production, and operational condition is constant, and the products obtained therefrom quality is high and stable, high-quality fire retardant can be become, and pharmaceutical grade can be reached.Reduced operational condition, temperature of reaction is low, and the waste heat of emitting in the time of can utilizing preparation ammoniacal liquor cuts down the consumption of energy, and saves a large amount of Freshwater resources.
Claims (6)
1, single stage method is produced the method for magnesium hydroxide, it is characterized in that: will contain the bittern of magnesium chloride and ammoniacal liquor is 1 according to the mol ratio of magnesium chloride and free ammonia: the mixed of 1.3-2.0, and mixture was reacted 5-30 minute in 45 ℃-90 ℃ environment, will obtain solid hydrogen magnesium oxide after the filtration of reaction solution process, washing, drying, the pulverizing.
2, single stage method according to claim 1 is produced the method for magnesium hydroxide, it is characterized in that: the reaction solution of bittern and ammoniacal liquor is at first once filtered, filtered liquid after once filtering prepares ammoniacal liquor through adding lime ammonia still process, filter cake after once filtering carries out secondary filtration after adding the water making beating again, the filter cake of secondary filtration makes solid hydrogen magnesium oxide again through super-dry, pulverizing.
3, single stage method according to claim 1 is produced the method for magnesium hydroxide, it is characterized in that: its proportioning is that the mol ratio according to magnesium chloride and free ammonia is 1 during the reaction of bittern and ammoniacal liquor: the mixed of 1.3-1.65, and mixture is reacted in 50 ℃-60 ℃ environment.
4, single stage method according to claim 1 and 2 is produced the method for magnesium hydroxide, and it is characterized in that: described filtration and washing process carry out in pressure filter.
5, single stage method according to claim 1 and 2 is produced the method for magnesium hydroxide, and it is characterized in that: described drying process is carried out in flash dryer.
6, single stage method according to claim 1 and 2 is produced the method for magnesium hydroxide, and it is characterized in that: described crushing process carries out in the fluidized bed type micronizer mill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01127343 CN1132784C (en) | 2001-08-21 | 2001-08-21 | One-step process of producing magnesium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01127343 CN1132784C (en) | 2001-08-21 | 2001-08-21 | One-step process of producing magnesium hydroxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1332117A CN1332117A (en) | 2002-01-23 |
| CN1132784C true CN1132784C (en) | 2003-12-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01127343 Expired - Fee Related CN1132784C (en) | 2001-08-21 | 2001-08-21 | One-step process of producing magnesium hydroxide |
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| CN (1) | CN1132784C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7771682B2 (en) | 2006-01-31 | 2010-08-10 | Council Of Scientific And Industrial Research | Process for the preparation of magnesia (MgO) from crude Mg (OH)2 |
| CN113233480A (en) * | 2021-06-29 | 2021-08-10 | 郭建文 | Magnesium refining slag recovery equipment and recovery process thereof |
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2001
- 2001-08-21 CN CN 01127343 patent/CN1132784C/en not_active Expired - Fee Related
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| CN1332117A (en) | 2002-01-23 |
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