CN1205120C - Method for producing magnesium from ludwigite - Google Patents

Method for producing magnesium from ludwigite Download PDF

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Publication number
CN1205120C
CN1205120C CN 03101382 CN03101382A CN1205120C CN 1205120 C CN1205120 C CN 1205120C CN 03101382 CN03101382 CN 03101382 CN 03101382 A CN03101382 A CN 03101382A CN 1205120 C CN1205120 C CN 1205120C
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China
Prior art keywords
boric acid
reaction
mineral
boron magnesium
boron
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Expired - Fee Related
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CN 03101382
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Chinese (zh)
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CN1456501A (en
Inventor
张有俊
胡月阳
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Xinyang Mineral Industry Co Ltd Dong
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Xinyang Mineral Industry Co Ltd Dong
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Priority to CN 03101382 priority Critical patent/CN1205120C/en
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Application granted granted Critical
Publication of CN1205120C publication Critical patent/CN1205120C/en
Anticipated expiration legal-status Critical
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  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The present invention relates to a method for producing boric acid from powder of boron and magnesium mineral. Pulverized mineral powder reacts in sulfuric acid with the concentration of 40 to 75% for 5 to 10 min, the pH is controlled to be between 1.5 and 4.5, and the reaction automatically rises in temperature to 160 DEG C at the most. After the reaction ends, stacked material is cooled to the room temperature, and the material is dry and solid. The dry and solid material is soaked in water, filtered, crystallized by cooling, separated and dried to obtain industrial boric acid conforming to the standard. Calcined powder of boron and magnesium mineral can also be used as raw material. Compared with the prior art, mineral with B2O3 content larger than 30% as well as mineral with B2O5 content larger than 12% can be used for preparing boric acid in the method of the present invention. Besides, the acidifying reaction time of mineral powder is greatly shortened, and acidified material becomes dry and is solidified without needing to treat waste acid and waste water, so that corrosion of reaction device is greatly reduced. The method of the present invention can particularly realize the purposes of small device and large capacity and provides conditions for the large-scale production of boric acid.

Description

Utilize boron magnesium ore deposit to produce the method for boric acid
Technical field
What the present invention relates to is the production technology of the compound of boracic and oxygen.
Background technology
Industrial boric acid is used for glass, sugared porcelain, ceramics in a large number, in the metallurgical industry as additive, fusing assistant; At chemical industry, then extensively as the raw material of sterilant, catalyzer, as sanitas, boric acid is one of basic raw material of producing other boron compounds in addition because it has preservative property.Industrial boric acid is to be added inorganic acid reaction and made by boron magnesium ore deposit.Normally the fine ore of boron is allocated to proper concn with mother liquor and water and sent in the acid hydrolysis tank, slowly add sulfuric acid after specified acid amount, stir certain hour, be warming up to 95~100 ℃, reaction 1~2h filters then, abandons out filter residue, filtrate is through cooling, crystallization, centrifugation, washing, drying and make boric acid (Chemicals handbook, inorganic chemicals industry handbook).Industrial scale processes is like this substantially.The production method of this industrial boric acid, very high to ingredient requirement, boron magnesium contains B in the ore deposit 2O 3>30%, so high-grade ore deposit really very little, so be difficult to be extensive use of.Have many irrational places in addition on the technology, as along with acidification reaction carries out, acidity descends and is exceedingly fast, and acidification reaction is incomplete, and the transformation efficiency of boron is not high to be very disadvantageous to producing; And the long raising that also affects throughput of reaction times; There is the processing of spent acid, waste water also to acquire a certain degree of difficulty again.
Summary of the invention
At the defective that above-mentioned prior art exists, the present invention will provide one to be raw material with common boron magnesium ore deposit, the operational path of efficient, simple manufacture boric acid.
As everyone knows, the boron magnesium in the boron rock changes into water-soluble boron, magnesium compound must react under the acidic conditions of low pH value and just can achieve the goal, and prior art can not satisfy this requirement in the whole process that transforms.Technical scheme of the present invention is: the broken particle of boron magnesium slag wants thin, need reach more than 100 orders, and making breeze in the reactor of whipping appts is arranged is stirring reaction 5~10min in 54~75% the mineral acid (as sulfuric acid) in concentration, controls reactant PH1.5~4.5.Reaction is heat release, and its temperature raises automatically, reaches as high as 160 ℃, and this state water of reaction generation down constantly evaporates, and makes mineral acid remain higher concentration, then reacts sustainable and proceeds to fully.Reaction is finished reactant (acid boron magnesium slag) is stacked cooling, and material is dried fully solid when reducing to room temperature, but and powdering, its water content<10%, this material can be with plastics bag or textile of chemical fibre bag splendid attire, transportation.During preparing boric acid, adopt general leaching legal system to get boric acid, be about to acid boron magnesium slag (solid boric acid, sal epsom) and place extraction vessel, leach with 90 ℃ of left and right sides hot water or preparing boric acid mother liquor, filter and remove residue then, filtrate are through overcooling, crystallization, centrifugation, drying and make the industrial boric acid of conformance with standard (GB/T538-90).
The also available ripe breeze of raw material boron magnesium slag, i.e. the breeze of boron magnesium ore deposit after roasting, its granularity is (〉=80 orders are all available) more slightly, and production effect is also fine.
Compared with prior art, the present invention's characteristics of giving prominence to are: (1) uses boron magnesium ore deposit ingredient requirement quite low: contain B 2O 3>30% ore deposit can be used, and contains B 2O 3Be lower than 30%, even 〉=15% lean ore can produce qualified boric acid; (2) acidification reaction technology is more reasonable: the water that utilizes reacting heat evaporation to generate, reaction is remained under higher acidity and the suitable temp carry out, thereby conversion reaction can be carried out fully; Make that thus acidification reaction speed is fast, the reaction times is short, and equipment capacity greatly improves, and can accomplish " the big production of skinny device "; Because reaction is fast, the time is short, and is less to the corrodibility of equipment, it is much simple that its rotproofing is wanted; In addition, the product of acidification reaction is a dry substance, does not produce waste water, spent acid, and environment is not polluted; Convenient and simple for operation on the technology.(3) because technologic improvement, make the utilization ratio of resource of boron improve, based on above reason, the present invention can make the boric acid production cost that obvious reduction has been arranged, the low institute of industrial scale acid and alkali long reaction time, throughput restricts, for condition has been created in industrial boric acid production maximization.
Embodiment
Example 1
The Kuandian boron ore powder, each component content is: CaO0.90%, MgO43.35%, Fe 2O 31.97%, Al 2O 30.82%, SiO 214.62%, B 2O 324.49%.The processing method of producing boric acid is:
(1) 100Kg,>the above-mentioned breeze of 100 purposes is added to and 60Kg water is housed, has in the reactor of whipping appts, adding concentration is 93% sulfuric acid 116Kg under stirring, reaction 5~10min, its PH is 2.0, reaction mass heats up automatically therebetween, is up to 150 ℃, and reacting rear material draws off stacks cooling, products solidifying becomes dry and comfortable powdery when reaching room temperature, water content<10%; (total amount 240Kg) B 2O 38.0%, MgSO 413.8%.
(2) above-mentioned dry and comfortable powder drops in the dessicator, carries out conventional general method leaching preparing boric acid process with 87~92 ℃ of water, slagging-off after filtration, filtrate crystallisation by cooling, centrifugation, oven dry and must meet GB/T538-90 by the boric acid sampling analysis.
Example 2
The ripe boron magnesium slag in the above-mentioned ore deposit of 100Kg (boron magnesium ore deposit is through roasting), granularity>80 orders, add and have in the reactor that is added with 110Kg water of agitator, adding concentration is 93% sulfuric acid 140Kg under stirring, reaction 5~10min, temperature of reaction reaches as high as 150 ℃, and reacting rear material draws off to stack and is cooled to room temperature, material is solidified into dry powder, moisture<10%.Preparing boric acid step such as example 1.
Example 3
100Kg contains B 2O 5Be 15% boron magnesium slag (>120 purpose particle diameter), add also have agitator and be added with in the reaction of 65Kg water, stir that to add concentration down be 93% sulfuric acid 90Kg, reaction 5~10min, its PH is 2.5, the Gao Kesheng of temperature of reaction reaches 130 ℃.The complete material of reaction draws off to stack and is cooled to room temperature, the dried meal that is solidified into of material, moisture<10%.Get boric acid with leaching legal system with example 1.
Example 4
Adding concentration in the reactor is 68.1% sulfuric acid 150Kg, will contain B under stirring 2O 330.49% boron magnesium slag (>120 order) adds wherein, and heating up naturally is up to 150 ℃, reaction 5~10min, and PH=2.0, reaction is finished discharging and is stacked cooling, does to the room temperature material to become sand shape admittedly.Leaching preparing boric acid method is with example 1.

Claims (3)

1, utilize boron magnesium ore deposit to produce the method for boric acid, it is characterized by:
Production technique is:
A, boron magnesium slag particle degree>100 orders are to react 5~10min in 54~75% sulfuric acid in concentration, control pH value 1.5~4.5, and temperature of charge rises automatically in the reaction, reaches as high as 160 ℃;
B, reaction are finished, and reaction product is stacked cooling, obtain dry substance, water-content<10% to room temperature;
C, dry substance add water extraction boric acid, after filtration, crystallisation by cooling, separation, oven dry and make boric acid.
2,, it is characterized by described boron magnesium slag and be the ripe breeze after the ore deposit roasting of boron magnesium according to the described method of utilizing boron magnesium ore deposit to produce boric acid of claim 1.
3, according to claim 1 or the 2 described methods of utilizing boron magnesium ore deposit to produce boric acid, it is characterized by described boron magnesium slag, its B 2O 3Content 〉=15%.
CN 03101382 2003-01-07 2003-01-07 Method for producing magnesium from ludwigite Expired - Fee Related CN1205120C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 03101382 CN1205120C (en) 2003-01-07 2003-01-07 Method for producing magnesium from ludwigite

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Application Number Priority Date Filing Date Title
CN 03101382 CN1205120C (en) 2003-01-07 2003-01-07 Method for producing magnesium from ludwigite

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CN1456501A CN1456501A (en) 2003-11-19
CN1205120C true CN1205120C (en) 2005-06-08

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100362115C (en) * 2005-12-06 2008-01-16 大连市中山区鑫阳矿业化工研究所 Separation method of boron, magnesium and iron in paigeite

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100460322C (en) * 2006-07-21 2009-02-11 大连市中山区鑫阳矿业化工研究所 Method for preparing boric acid from borax
CN101549876B (en) * 2009-05-15 2011-05-25 东北大学 Method for producing boric acid and co-produce magnesium hydrate and calcium sulphate by utilizing boron-rich slag

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100362115C (en) * 2005-12-06 2008-01-16 大连市中山区鑫阳矿业化工研究所 Separation method of boron, magnesium and iron in paigeite

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