CN105621460A - Production method of anhydrous magnesium salt - Google Patents

Production method of anhydrous magnesium salt Download PDF

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Publication number
CN105621460A
CN105621460A CN201511026476.3A CN201511026476A CN105621460A CN 105621460 A CN105621460 A CN 105621460A CN 201511026476 A CN201511026476 A CN 201511026476A CN 105621460 A CN105621460 A CN 105621460A
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Prior art keywords
magnesium salt
acid
solution
anhydrous magnesium
production method
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CN201511026476.3A
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Chinese (zh)
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王丰登
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Individual
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/32Phosphates of magnesium, calcium, strontium, or barium
    • C01B25/34Magnesium phosphates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/26Magnesium halides
    • C01F5/30Chlorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/40Magnesium sulfates
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • C01P2006/82Compositional purity water content

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)

Abstract

The invention discloses a production method of anhydrous magnesium salt. The method comprises the following steps of (1) adding acid and magnesium oxide into a reaction vessel; then, adding water as a reaction medium; mixing and stirring the materials for reaction to obtain an impurity-containing magnesium salt coarse solution with the temperature being 60 to 130 DEG C; (2) filtering the impurity-containing magnesium salt coarse solution obtained in the first step when the solution is still hot so as to remove impurities, and obtaining a magnesium salt solution being 50 to 120 DEG C; (3) heating the magnesium salt solution obtained in the second step, and maintaining the temperature of 50 to 150 DEG C to form a solution; (4) performing spray drying on the solution obtained in the third step, and after the drying, forming magnesium salt containing 0.5 to 4 percent of free water and 2 to 25 percent of crystal water; (5) drying the magnesium salt obtained in the fourth step to remove the rest water, and obtaining the anhydrous magnesium salt with the water content being less than 2 percent. The production method has the advantages that the work procedures are reduced; the equipment is reduced; the energy consumption is reduced; the goal of reducing the production cost is achieved; the product cost is low; great promotion effects are achieved on industrial production.

Description

The production method of a kind of anhydrous magnesium salt
Technical field
The present invention relates to magnesium salt compound production technical field, it is specifically related to the production method of a kind of anhydrous magnesium salt.
Background technology
Magnesium salt is had many uses, and as fertilizer application, it can not only provide magnesium elements, and can chessom. Anhydrous magnesium salt is content height compared with the advantage of other magnesium salt, not easily gets damp. What usage quantity was bigger is anhydrous magnesium sulfate salt. In livestock industry, magnesium salt can as the supplement of magnesium in feed manufacturing. The factor that magnesium is indispensable when being participate in livestock and poultry body making bone process and Muscle contraction, is the activator of multiple enzyme in livestock and poultry body, the substance metabolism in livestock and poultry body and neural function is played an important role. In industrial application, anhydrous magnesium salt is applied to the additive synthesis of ABS and polyvinyl chloride resin, papermaking, dyeing industry etc.; In addition for Industrial Waste Water Treatments, waste liquid sewage is played condensation and sedimentation effect so that it is reach pollution exhaust criteria. Leather industry is done weighting agent and strengthens thermotolerance; Printing and dyeing can be used as fabric contaminates agent, weighting agent, magnesium dye agent; The fire retardant of the plastics such as acrylate resin it is used as in fire-retardant material. Anhydrous magnesium salt can be used for product synthesis that water-content can not be too high and mix, for can be used for siccative and dewatering agent in chemical industry, for carefully thin cotton, the silk of printing and dyeing, as the cotton weighting agent of silk and the filler of kapok goods. In pharmacy, magnesium sulfate is processed as the medicines such as cathartic, anticonvulsive drug, Magnesium Trisilicate, Meleumycinum, acetylspiramycin and flesh former times. Anhydrous magnesium salt also can be used for producing fresh yeast, monosodium glutamate, artificial snow, beverage, mineral water, bath salt, washing composition, shampoo etc., and in foodstuffs industry, magnesium salt is used for lactic acid, monosodium glutamate etc.
Existing anhydrous magnesium salt production technology, after mostly adopting acid, water and magnesia powder hybrid reaction, slightly cools, refilters, then be cooled to normal temperature, crystallization, and crystallization magnesium salt is through heat temperature raising, more multistage calcination produces. This technical process operation is long, and processing units is many, and post is many, and reaction heat can not be applied, and increases energy consumption. Costly various, cost height.
The information being disclosed in this background section only is intended to increase the understanding of the general background to the present invention, and should not be regarded as admitting or imply that this information structure has been prior art that persons skilled in the art are known in any form.
Summary of the invention
The present invention, for solving the problems of the technologies described above, invents the production method of a kind of anhydrous magnesium salt, it is intended to realize producing brief operation in anhydrous magnesium salt process, shorten the production time, reduce energy consumption, improving the object of cost.
For achieving the above object, technical scheme provided by the invention is as follows:
A production method for anhydrous magnesium salt, comprises the following steps:
(1) acid and magnesium oxide being joined in reactor, then add water as reaction medium, mix and blend reacts, and obtains the thick solution of magnesium salt containing impurity, solution temperature 60��130 DEG C;
(2) the thick solution filtered while hot of magnesium salt step (1) gained containing impurity removes impurity, obtains the magnesium salt solution of 50��120 DEG C;
(3) in step (2) gained magnesium salt solution heat and keep temperature 50��150 DEG C formed solution;
(4) step (3) gained solution is carried out spraying dry, after dry, form the magnesium salt of 2��25% crystal water containing 0.5��4% free water;
(5) in step (4) gained magnesium salt again drying remove residual moisture, obtain the anhydrous magnesium salt of moisture less than 2%.
Preferably, described acid is at least one in sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid, carbonic acid, ureasulfuric acid, Ureaphil, gluconic acid, citric acid, lactic acid, oxysuccinic acid, tartrate, amino acid.
Preferably, the acid added in step (1) and oxidation magnesium amount are mol ratio acid: magnesium oxide=0.9��3:1.
Preferably, the drying described in step (5) is drum dried or fluidised bed drying.
Compared with prior art, the present invention has following useful effect:
Production method of the present invention eliminates crystallisation by cooling operation, the centrifugal separation process of magnesium salt, apply reaction heat to greatest extent, reduction reaction, filtration need moisture, directly remove major part freedom or crystallization moisture by spraying dry of heating, then become anhydrous magnesium salt through follow-up drying. Operation reduces, and equipment reduces, and energy consumption reduces, and reaches and reduces production cost object, and product cost is low, has bigger promoter action in industrial production.
Embodiment
It is described in detail below in conjunction with embodiment, it should be understood that protection scope of the present invention is not by the restriction of embodiment.
Embodiment 1
(1) according to mol ratio acid: magnesium oxide=1:1 takes sulfuric acid, magnesia powder, sulfuric acid and magnesia powder are joined mix and blend reaction in reactor, obtains the thick solution of magnesium salt containing impurity, solution temperature 60 DEG C;
(2) the thick solution filtered while hot of magnesium salt step (1) gained containing impurity removes impurity, obtains the magnesium salt solution of 50 DEG C;
(3) in step (2) gained magnesium salt solution again through heat and keep temperature 50 DEG C formed solution;
(4) step (3) gained solution is delivered to spray-drying tower and carries out spraying dry, after dry, form the magnesium salt of 2��25% crystal water containing 0.5��4% free water;
(5) in step (4), gained magnesium salt removes residual moisture through drum dried kiln drying is dry again, obtains the anhydrous magnesium salt of moisture less than 2%.
Embodiment 2
(1) according to mol ratio acid: magnesium oxide=3:1 takes phosphoric acid, magnesia powder, sulfuric acid and magnesia powder are joined mix and blend reaction in reactor, obtains the thick solution of magnesium salt containing impurity, solution temperature 130 DEG C;
(2) the thick solution filtered while hot of magnesium salt step (1) gained containing impurity removes impurity, obtains the magnesium salt solution of 120 DEG C;
(3) in step (2) gained magnesium salt solution again through heat and keep temperature 150 DEG C formed solution;
(4) step (3) gained solution is delivered to spray-drying tower and carries out spraying dry, after dry, form the magnesium salt of 2��25% crystal water containing 0.5��4% free water;
(5) in step (4), gained magnesium salt removes residual moisture through fluidised bed drying again, obtains the anhydrous magnesium salt of moisture less than 2%.
Embodiment 3
(1) according to mol ratio acid: magnesium oxide=2:1 takes ureasulfuric acid, citric acid, the mixture of oxysuccinic acid, magnesia powder, sulfuric acid and magnesia powder are joined mix and blend reaction in reactor, obtains the thick solution of magnesium salt containing impurity, solution temperature 95 DEG C;
(2) the thick solution filtered while hot of magnesium salt step (1) gained containing impurity removes impurity, obtains the magnesium salt solution of 85 DEG C;
(3) in step (2) gained magnesium salt solution again through heat and keep temperature 100 DEG C formed solution;
(4) step (3) gained solution is delivered to spray-drying tower and carries out spraying dry, after dry, form the magnesium salt of 2��25% crystal water containing 0.5��4% free water;
(5) in step (4), gained magnesium salt removes residual moisture through fluidised bed drying again, obtains the anhydrous magnesium salt of moisture less than 2%.
Embodiment 4
(1) according to mol ratio acid: magnesium oxide=0.9:1 takes hydrochloric acid, magnesia powder, sulfuric acid and magnesia powder are joined mix and blend reaction in reactor, obtains the thick solution of magnesium salt containing impurity, solution temperature 110 DEG C;
(2) the thick solution filtered while hot of magnesium salt step (1) gained containing impurity removes impurity, obtains the magnesium salt solution of 95 DEG C;
(3) in step (2) gained magnesium salt solution again through heat and keep temperature 110 DEG C formed solution;
(4) step (3) gained solution is delivered to spray-drying tower and carries out spraying dry, after dry, form the magnesium salt of 2��25% crystal water containing 0.5��4% free water;
(5) in step (4), gained magnesium salt removes residual moisture through drum dried kiln drying is dry again, obtains the anhydrous magnesium salt of moisture less than 2%.
The aforementioned description to the concrete exemplary of the present invention is to illustrate and the object of illustration. These descriptions not want to be defined as the present invention disclosed precise forms, and obviously, according to above-mentioned instruction, it is possible to carry out much changing and change. The object exemplary embodiment selected and describe is to explain the certain principles of the present invention and practical application thereof, so that the technician of this area can realize and utilize the various different exemplary of the present invention and various different selection and change. The scope of the present invention is intended to be limited by claim book and equivalents thereof.

Claims (4)

1. the production method of an anhydrous magnesium salt, it is characterised in that, comprise the following steps:
(1) acid and magnesium oxide being joined in reactor, then add water as reaction medium, mix and blend reacts, and obtains the thick solution of magnesium salt containing impurity, solution temperature 60��130 DEG C;
(2) the thick solution filtered while hot of magnesium salt step (1) gained containing impurity removes impurity, obtains the magnesium salt solution of 50��120 DEG C;
(3) in step (2) gained magnesium salt solution heat and keep temperature 50��150 DEG C formed solution;
(4) step (3) gained solution is carried out spraying dry, after dry, form the magnesium salt of 2��25% crystal water containing 0.5��4% free water;
(5) in step (4) gained magnesium salt again drying remove residual moisture, obtain the anhydrous magnesium salt of moisture less than 2%.
2. the production method of anhydrous magnesium salt according to claim 1, it is characterised in that: described acid is at least one in sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid, carbonic acid, ureasulfuric acid, Ureaphil, gluconic acid, citric acid, lactic acid, oxysuccinic acid, tartrate, amino acid.
3. the production method of anhydrous magnesium salt according to claim 1, it is characterised in that: the acid added in step (1) and oxidation magnesium amount are mol ratio acid: magnesium oxide=0.9��3:1.
4. the production method of anhydrous magnesium salt according to claim 1, it is characterised in that: the drying described in step (5) is drum dried or fluidised bed drying.
CN201511026476.3A 2015-12-31 2015-12-31 Production method of anhydrous magnesium salt Pending CN105621460A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106083565A (en) * 2016-06-06 2016-11-09 宁乡新阳化工有限公司 The production method of magnesium lactate
CN113956152A (en) * 2021-10-21 2022-01-21 上海凝璇企业管理合伙企业(有限合伙) Preparation method of alpha-ketoglutaric acid magnesium salt

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1118785A (en) * 1994-05-07 1996-03-20 中国人民解放军空军上海第一医院 Magnesium gluconate for medicine use and its preparation method for oral liquor
CN101939282A (en) * 2008-02-08 2011-01-05 普拉克生化公司 Metal lactate powder and method for preparation
CN102285877A (en) * 2010-06-17 2011-12-21 陆生杰 Method for producing magnesium citrate
CN103708509A (en) * 2013-12-20 2014-04-09 杨海基 Method for producing magnesium sulfate monohydrate by using spray drying process
CN104355989A (en) * 2014-10-29 2015-02-18 宜兴市前成生物有限公司 Method for preparing magnesium malate
CN104447272A (en) * 2014-11-14 2015-03-25 宁乡新阳化工有限公司 Production method of magnesium citrate anhydrous

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1118785A (en) * 1994-05-07 1996-03-20 中国人民解放军空军上海第一医院 Magnesium gluconate for medicine use and its preparation method for oral liquor
CN101939282A (en) * 2008-02-08 2011-01-05 普拉克生化公司 Metal lactate powder and method for preparation
CN102285877A (en) * 2010-06-17 2011-12-21 陆生杰 Method for producing magnesium citrate
CN103708509A (en) * 2013-12-20 2014-04-09 杨海基 Method for producing magnesium sulfate monohydrate by using spray drying process
CN104355989A (en) * 2014-10-29 2015-02-18 宜兴市前成生物有限公司 Method for preparing magnesium malate
CN104447272A (en) * 2014-11-14 2015-03-25 宁乡新阳化工有限公司 Production method of magnesium citrate anhydrous

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106083565A (en) * 2016-06-06 2016-11-09 宁乡新阳化工有限公司 The production method of magnesium lactate
CN113956152A (en) * 2021-10-21 2022-01-21 上海凝璇企业管理合伙企业(有限合伙) Preparation method of alpha-ketoglutaric acid magnesium salt

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Application publication date: 20160601