CN101850994A - Method for preparing flame-retardant grade magnesium hydroxide - Google Patents
Method for preparing flame-retardant grade magnesium hydroxide Download PDFInfo
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- CN101850994A CN101850994A CN 201010209952 CN201010209952A CN101850994A CN 101850994 A CN101850994 A CN 101850994A CN 201010209952 CN201010209952 CN 201010209952 CN 201010209952 A CN201010209952 A CN 201010209952A CN 101850994 A CN101850994 A CN 101850994A
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Abstract
The invention discloses a method for preparing flame-retardant grade magnesium hydroxide. The method comprises: A1, a synthetic reaction step, in which magnesium sulfate is used as a raw material and sodium hydroxide is used as a transforming agent, and a synthetic reaction is performed in a synthesizer; A2, an activating step, in which a precipitator and an active agent are added into the mixed solution obtained by the step A1 for activation, after activation, press filtration is performed in a high-pressure automatic membrane press-filter, the obtained products are washed by deionized water and thus A-type magnesium hydroxide is obtained; A3, a modification step, in which high-temperature modification of the A-type magnesium hydroxide is performed, the modified mixed solution is filtered by the high-pressure automatic membrane press-filter, the obtained products are washed by deionized water, and thus, B-type magnesium hydroxide is obtained; and A4, a drying-crushing step, in which the drying and crushing of the B-type magnesium hydroxide are performed, and thus, the finished products of the flame-retardant grade magnesium hydroxide are obtained.
Description
Technical field
The present invention relates to chemical field, in particular a kind of manufacture method of flame-proof magnesium hydroxide.
Background technology
China is magnesium resource big country, and western salt lake magnesium resource is particularly abundant.Salt lake, Qaidam magnesium salts reserves are up to 48.1 hundred million tons, be the excellent raw material resources of high-end magnesium salts products production, simultaneously, annual discharging higher-grade sal epsom, magnesium chloride in producing boric acid and potash fertilizer process, and its utilization ratio has only about 2%, not only cause the wasting of resources, also form " magnesium evil ", make potential magnesium resource advantage fail to be converted into considerable economic and social benefit.Its exploitation still is in the rudimentary starting stage, and from the production capacity of magnesium hydroxide: the production capacity of China's magnesium hydroxide is very low at world's portion, and the gap of comparing them with demand will be expansion trend in from now on several years; From importing and exporting: outlet mostly is ordinary hydrogen magnesium oxide and magnesium oxide, and ultra-fine and even nanometric magnesium hydroxide is mainly by import, and bigger with the price rises amplitude that reduces the market magnesium hydroxide in particle footpath.So, be to have the vast market future for the research and development of ultra-fine and even nanometric magnesium hydroxide.But the salt lake magnesium resource will be carried out large-scale development, still exists the scientific and technological problem of many-sided key, and they have become the technology " bottleneck " that the restriction salt lake resources develops to extensive industrialization direction.Super-refinement along with magnesium hydroxide particle: separation, washing etc. bring difficulty to post-processing operation; Have special appearance simultaneously, the surface modification that organises magnesium hydroxide then needs the special preparation technology just can meet the demands.Wherein: the scientific and technological problems such as control of solid-liquid separation, modification, dispersiveness and crystal morphology are again in the engineering amplification process, simplify technological process, reduce production costs, improve the cost performance of flame retardant of magnesium hydroxide, strengthen its market competitive power, unavoidable key technical problem.
Therefore, there is defective in prior art, needs to improve.
Summary of the invention
Technical problem to be solved by this invention is.
Technical problem to be solved by this invention is at the deficiencies in the prior art, provides a kind of utilization to utilize the sal epsom of industrial production boric acid or potash fertilizer by-product to be raw material, manufactures the method for flame-proof magnesium hydroxide.
Technical scheme of the present invention is as follows:
A kind of manufacture method of flame-proof magnesium hydroxide may further comprise the steps: A1: the building-up reactions step is a raw material with sal epsom, is transforming agent with sodium hydroxide, carries out building-up reactions in synthesizer; A2: activation step, adding precipitation agent and activator activate in the mixed solution that steps A 1 obtains, and activation finishes after the press filtration of high pressure automatic diaphragm pressure filter uses the deionized water washing to obtain A type magnesium hydroxide; A3: modification procedure, through high temperature modified, the mixed solution after the modification filters by high pressure automatic diaphragm pressure filter again with described A type magnesium hydroxide, uses the deionized water washing, makes the Type B magnesium hydroxide; A4: the drying and crushing step, with described Type B magnesium hydroxide process drying and crushing, the flame-proof magnesium hydroxide finished product that can obtain.The half-finished filtration problem of magnesium hydroxide is a great problem that perplexs in the industry always, the filtration factor of whizzer is very big, but there is not good filter cloth, the centrifuge speed of 1000mm reached before 600 rev/mins, substantially the solid-liquid separation of having no idea to realize, when rotating speed surpassed 800-1000 rev/min, the leakage filter was just very serious.Homemade full-automatic high-pressure diaphragm filter press then is easy to finish the operation of this operation when handling the filtration of magnesium hydroxide, filter, wash, drain the requirement that can satisfy technology, and can realize automated operation.
Described manufacture method, sal epsom described in the described steps A 1 is for producing the sal epsom of by-product in boric acid or the potash fertilizer technology.
Described manufacture method, synthetic reaction condition is in the described steps A 1: temperature of reaction 100-130 degree, the reaction times was controlled in 120 minutes, and the rotating speed of synthesizer changes for per minute 250-350.
Described manufacture method, described synthesizer rotating speed are that per minute 300 changes.Described manufacture method is characterized in that, properties-correcting agent described in the steps A 2 is fatty acid sodium, and described precipitation agent is a polyacrylamide.
Described manufacture method, the drying and crushing method is in the steps A 4: through the prebake of bidirectional screw drying machine, pulverize and enter the high velocity air drying machine again and thoroughly dry.The drying of magnesium hydroxide products is a technical barrier, tradition generally is to adopt cyclone drying, the main drawback of cyclone drying is exactly very low of thermo-efficiency, characteristics such as the throughput of equipment is little, and heat energy loss is big, and the loss of material is big, adopt the bidirectional screw drying machine to carry out preliminary drying, the advantage of bidirectional screw drying machine not only can play the effect of prebake but also can play the effect of pre-mixing precomminution, and energy consumption can drop to the moisture of magnesium hydroxide below 4% by 10% than the low efficiency height.
1. this technology process route is simple and clear, invests for a short time, does not have industrial effluent to efflux, and suitability for industrialized production realizes very much.
2. production cost is low, owing to do not have effluxing of waste liquid in the technology, realizes the closed cycle of material, so this explained hereafter cost is very low.
3. technic index control is simple, and this technology can effectively realize the automation integrated control of technological operation, and automated operation is very strong.
4. the quality of product---whiteness purity particle diameter controllability is strong.
5. can improve the market competitiveness of boronation industrial and commercial bank industry effectively by the added value that improves by-product.
There is following beneficial effect with the present invention that compares of bittern ammonia process:
(1) quality index: with the quality product of this explained hereafter near or reached the index of bittern ammonia process, some index even be higher than the bittern ammonia process.
(2) production cost: compare with the various processing methodes of bittern ammonia process and other, this Process is a less expensive.One ton of liquefied ammonia price is about 3400 yuan, and 1 ton of caustic soda has only about 1800 yuan.So employing the inventive method, Technology are both economical worthwhile, what need special proposition is generally not use bittern ammonia process technology in the world.
(3) byproduct reclaims.Byproduct with the production of bittern ammonia process is an ammonium chloride, or calcium chloride, the cost of product generally will surpass more than 8000 yuan if ammonium chloride then produces then, if calcium chloride then technology drop into and huge ammonia still process will be arranged, inhale ammonia, also will there be the recovery system of calcium chloride in system, system will add calcium hydroxide, also being very to calculate on the energy consumption cost, is sal glauberi with the byproduct of sal epsom soda processes, reclaims simply.
(4) environmental problem.Ammonia nitrogen is the material of national strict limiting emission, so the concentrated recovery of the ammonium chloride mother liquor that reaction produces is a very big problem, in a lot of local cost recovery possibly greater than selling price, in fact a lot of magnesium oxide manufacturing enterprises all are in discharging violating the regulations at present, next is the environmental problem of production process, the production process of bittern ammonia process has very dense ammonia stink, has a strong impact on the healthy of direct labor, solve the very big possibly dynamics of environmental problem.
(5) investment contrast: for large batch of production, it is minimum adopting the investment of sal epsom soda processes Technology.To produce ten thousand tons of magnesium hydroxide production lines per year is example, and the investment of only supporting synthetic ammonia process will nearly hundred million yuan.And if adopt the investment of sal epsom soda processes Technology just much of that with the remnant of synthetic ammonia.
Owing to these these reasons, the production that China adopts ammonia process to produce magnesium hydroxide manufacturer did not have substantial development in recent years, and the one, cost is too high can't realize profit on sales, loss occurs, the 2nd, technology is had no idea perfect.The buying of liquefied ammonia and the buying of milk of lime also have problems such as discharging any waste liquor not have good terms of settlement, are difficult to further develop, and this has had a strong impact on the utilization of salt lake magnesium resource.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is Mg of the present invention (OH)
2Particle (nano level) agent (micron order) the adsorption process synoptic diagram that is modified;
Fig. 3 is the magnesium hydroxide laser scanning electron microscope film making that the present invention makes;
Fig. 4 is the magnesium hydroxide laser scanning electron microscope film making that the present invention makes.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
As shown in Figure 1, the invention provides a kind of manufacture method of flame-proof magnesium hydroxide, may further comprise the steps: A1: the building-up reactions step is a raw material with sal epsom, is transforming agent with sodium hydroxide, carries out building-up reactions in synthesizer; A2: activation step, adding precipitation agent and activator activate in the mixed solution that steps A 1 obtains, and activation finishes after the press filtration of high pressure automatic diaphragm pressure filter uses the deionized water washing to obtain A type magnesium hydroxide; A3: modification procedure, described A type magnesium hydroxide process is high temperature modified, for example, under 16 kilograms of pressure, temperature is 200 ℃, and modification is 2 hours under the rotating speed that per minute 300 changes, and the mixed solution after the modification filters by high pressure automatic diaphragm pressure filter again, the washing of use deionized water makes the Type B magnesium hydroxide; A4: the drying and crushing step, with described Type B magnesium hydroxide process drying and crushing, the flame-proof magnesium hydroxide finished product that can obtain.The half-finished filtration problem of magnesium hydroxide is a great problem that perplexs in the industry always, the filtration factor of whizzer is very big, but there is not good filter cloth, the centrifuge speed of 1000mm reached before 600 rev/mins, substantially the solid-liquid separation of having no idea to realize, when rotating speed surpassed 800-1000 rev/min, the leakage filter was just very serious.Homemade full-automatic high-pressure diaphragm filter press then is easy to finish the operation of this operation when handling the filtration of magnesium hydroxide, filter, wash, drain the requirement that can satisfy technology, and can realize automated operation.
The particle and the plane of crystal of transforming agent sodium hydroxide have bonding action, on different planes of crystal selective adsorption can take place, make some crystal face growth retardation, reduce the speed of growth, and relative growth rate is accelerated on other crystal faces, thereby has changed crystal morphology.Transforming agent can change the surface energy of medium, and from crystal growth molecular dynamics theoretical analysis, transforming agent sodium hydroxide has changed the energy of process of growth, has changed the saturation ratio of solution.The solution degree of supersaturation all has very big influence to crystalline growth velocity, quality, density, specific surface area, crystal morphology etc.
Preferably, in the above-mentioned manufacture method, sal epsom described in the described steps A 1 is for producing the sal epsom of by-product in boric acid or the potash fertilizer technology.
Preferably, in the above-mentioned manufacture method, synthetic reaction condition is in the described steps A 1: temperature of reaction 100-130 degree, and the reaction times was controlled in 120 minutes, and the rotating speed of synthesizer changes for per minute 250-350.
Preferably, in the above-mentioned manufacture method, described synthesizer rotating speed is that per minute 300 changes.Described manufacture method is characterized in that, properties-correcting agent described in the steps A 2 is fatty acid sodium, and described precipitation agent is a polyacrylamide.The application purpose of properties-correcting agent fatty acid sodium mainly contains: organic modification, dispersion, complete crystal formation and solid-liquid separation.As shown in Figure 2, be modified agent fatty acid sodium (micron order) adsorption process synoptic diagram as can be seen by Mg (OH) 2 particles (nano level), add the necessity of properties-correcting agent, simultaneously the mutual composite importance of multiple properties-correcting agent as nano particle " carrier " effect in the liquid phase production process.
Preferably, in the above-mentioned manufacture method, the drying and crushing method is in the steps A 4: through the prebake of bidirectional screw drying machine, pulverize and enter the high velocity air drying machine again and thoroughly dry.The drying of magnesium hydroxide products is a technical barrier, tradition generally is to adopt cyclone drying, the main drawback of cyclone drying is exactly very low of thermo-efficiency, characteristics such as the throughput of equipment is little, and heat energy loss is big, and the loss of material is big, adopt the bidirectional screw drying machine to carry out preliminary drying, the advantage of bidirectional screw drying machine not only can play the effect of prebake but also can play the effect of pre-mixing precomminution, and energy consumption can drop to the moisture of magnesium hydroxide below 4% by 10% than the low efficiency height.
The magnesium hydroxide laser scanning electron microscope film making that Fig. 3 and Fig. 4 obtain for present embodiment, hexagonal crystallization sheet is complete as can be seen from the picture.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (6)
1. the manufacture method of a flame-proof magnesium hydroxide is characterized in that, may further comprise the steps: A1: the building-up reactions step is a raw material with sal epsom, is transforming agent with sodium hydroxide, carries out building-up reactions in synthesizer; A2: activation step, adding precipitation agent and activator activate in the mixed solution that steps A 1 obtains, and activation finishes after the press filtration of high pressure automatic diaphragm pressure filter uses the deionized water washing to obtain A type magnesium hydroxide; A3: modification procedure, through high temperature modified, the mixed solution after the modification filters by high pressure automatic diaphragm pressure filter again with described A type magnesium hydroxide, uses the deionized water washing, makes the Type B magnesium hydroxide; A4: the drying and crushing step, with described Type B magnesium hydroxide process drying and crushing, the flame-proof magnesium hydroxide finished product that can obtain.
2. manufacture method according to claim 1 is characterized in that, sal epsom described in the described steps A 1 is for producing the sal epsom of boric acid or potash fertilizer by-product.
3. manufacture method according to claim 1 is characterized in that, synthetic reaction condition is in the described steps A 1: temperature of reaction 100-130 degree, and the reaction times was controlled in 120 minutes, and the rotating speed of synthesizer changes for per minute 250-350.
4. manufacture method according to claim 4 is characterized in that, described synthesizer rotating speed is that per minute 300 changes.
5. manufacture method according to claim 1 is characterized in that, properties-correcting agent is fatty acid sodium described in the described steps A 2, and described precipitation agent is a polyacrylamide.
6. manufacture method according to claim 1 is characterized in that, the drying and crushing method is in the described steps A 4: prebake, pulverizing through the bidirectional screw drying machine enter the oven dry of high velocity air drying machine again.
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| CN 201010209952 CN101850994B (en) | 2010-06-28 | 2010-06-28 | Method for preparing flame-retardant grade magnesium hydroxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303879A (en) * | 2011-07-29 | 2012-01-04 | 武汉工程大学 | Method for preparing magnesium hydroxide by utilizing light calcined dolomite |
| CN102491381A (en) * | 2011-12-16 | 2012-06-13 | 江苏艾特克阻燃材料有限公司 | Preparation method for flame retardant magnesium hydroxide |
| CN103523808A (en) * | 2013-09-27 | 2014-01-22 | 中盐制盐工程技术研究院 | Method for producing chloride-free magnesium hydroxide flame retardant from magnesia |
| CN113881445A (en) * | 2021-09-29 | 2022-01-04 | 白银康宝新型节能建材有限责任公司 | Preparation method of magnesium-based flame-retardant material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1541943A (en) * | 2003-11-08 | 2004-11-03 | 山东海化集团有限公司 | Preparing method for superfine highly dispersed magnesium hydroxide |
| CN101544388A (en) * | 2008-03-26 | 2009-09-30 | 南京理工大学 | Method for preparing modified sheeted nanometer magnesium hydroxide |
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2010
- 2010-06-28 CN CN 201010209952 patent/CN101850994B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1541943A (en) * | 2003-11-08 | 2004-11-03 | 山东海化集团有限公司 | Preparing method for superfine highly dispersed magnesium hydroxide |
| CN101544388A (en) * | 2008-03-26 | 2009-09-30 | 南京理工大学 | Method for preparing modified sheeted nanometer magnesium hydroxide |
Non-Patent Citations (3)
| Title |
|---|
| 《化工新型材料》 20020731 吴崇浩等 纳米微粒表面修饰的研究进展 1-5 1-6 第30卷, 第7期 2 * |
| 《过程工程学报》 20050228 向兰等 氢氧化镁在聚丙烯酰胺体系中的聚沉行为 58-61 1-6 第5卷, 第1期 2 * |
| 《镁化合物生产与应用》 20040331 胡庆福 第18章 阻燃级氢氧化镁 315-326 1-6 , 1 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303879A (en) * | 2011-07-29 | 2012-01-04 | 武汉工程大学 | Method for preparing magnesium hydroxide by utilizing light calcined dolomite |
| CN102491381A (en) * | 2011-12-16 | 2012-06-13 | 江苏艾特克阻燃材料有限公司 | Preparation method for flame retardant magnesium hydroxide |
| CN102491381B (en) * | 2011-12-16 | 2014-06-25 | 江苏艾特克阻燃材料有限公司 | Preparation method for flame retardant magnesium hydroxide |
| CN103523808A (en) * | 2013-09-27 | 2014-01-22 | 中盐制盐工程技术研究院 | Method for producing chloride-free magnesium hydroxide flame retardant from magnesia |
| CN113881445A (en) * | 2021-09-29 | 2022-01-04 | 白银康宝新型节能建材有限责任公司 | Preparation method of magnesium-based flame-retardant material |
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