CN102992338A - Method for producing boric acid through continuous automatic crystallization - Google Patents
Method for producing boric acid through continuous automatic crystallization Download PDFInfo
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- CN102992338A CN102992338A CN2013100003819A CN201310000381A CN102992338A CN 102992338 A CN102992338 A CN 102992338A CN 2013100003819 A CN2013100003819 A CN 2013100003819A CN 201310000381 A CN201310000381 A CN 201310000381A CN 102992338 A CN102992338 A CN 102992338A
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Abstract
The invention belongs to the technical field of boric acid production and particularly relates to a method for producing boric acid through continuous automatic crystallization. The method includes: acidizing boric ore, filtering to remove impurities, cooling and crystallizing, filtering to remove mother solution, and drying and dehydrating to obtain boric acid. The method is characterized in that a cooling crystallization process is divided into four processes of cooling, crystallizing, floating crystal negative-pressure draining and water-adding heating secondary dissolution, cooling temperature of the cooling process is 22-26 DEC G, negative pressure in the floating crystal negative-pressure draining process is at 0.2-0.4Pa, heating temperature in the water-adding heating secondary dissolution process is 70-80 DEG C, and PH value of sulfuric acid for solution is regulated to 2.95-3.05. The method has the advantage that the production process achieves efficient and continuous automatic crystallization, production capacity and automation degree of a device are improved, boric acid crystals with large particle size and ideal crystal form can be obtained in production, product quality is stabilized at 99.9%, energy consumption is reduced, and problems of wall scaling and floating crystal are solved.
Description
One, technical field:The invention belongs to the production technical field of boric acid, particularly the method for boric acid is produced in a kind of continuous and automatic crystallization.
Two, background technology:
The at present production of boric acid both at home and abroad is because various countries' boron resource is different, and its method of producing boric acid also is not quite similar, but take acid system as main, makes the boron in the raw material be converted into boric acid, separates out boric acid through crystallisation by cooling again.The crystallisation process of boric acid is a very important productive unit in process of production, and the transformation efficiency of boron and the quality of product are just played crucial effect.Produce boric acid both at home and abroad and still adopt the intermittent type crystallization production technology, the crystallizer of employing mostly is stainless steel or is lined with the vertical crystallizer that the ordinary steel in the lead is made, and shape is like the tubular pot with taper round bottom and deadend.In order to increase cooling area and to reduce the consumption of refrigerant, the cooling coil of plumbous system or steel is housed in crystallizer usually or cooling jacket is housed outside production equipment, when operate continuously as underground water and the filtrate counter-current operation of refrigerant.Rotating speed also be housed be the per minute 60 right paddle stirrer that turns left in these crystallizers.The advantage of this boric acid crystallization production process is that device structure is simple, and is easy to manufacture.But also there are a lot of shortcomings in the crystallization production process of this mode: periodical operation, and throughput is little; The low conversion rate of boron only can reach about 80%; It is less, irregular that the crystal formation of producing boric acid shows as particle more, and quality product is not high; Each crystallizer needs a cover whipping device, and the power of motor that needs is larger, and power consumption is high; In process of production because inhomogeneous cooling is even, the very easily long-pending knot of crystal is on coiled pipe or crystallization tank skin and reduce heat transfer efficiency, and not only heat exchange effect is low, and must often remove to improve operation; Boric acid is in crystallisation process in addition, and crystallizer top is understood some very small crystal foam and produced, and is namely floating brilliant, because the floating brilliant bad control of generation, floating brilliant small but can not grow up again, will have influence on the crystallisation process of boric acid, also can affect the service efficiency of crystallizer.
This step crystallization production technology can not meet the needs of production at present, through investigation, boric acid continuous and automatic crystallization production technology at present at home and abroad or a blank, in order to change this disadvantageous passive situation, we carry out research of technique, have finished the research work to boric acid continuous and automatic crystallization production technology project.
Three, summary of the invention:
The objective of the invention is for above shortcomings in the prior art, and the method that boric acid is produced in a kind of continuous and automatic crystallization of research and design, the advantage of the method is: one. production technique has realized efficiently, the continuous and automatic crystallization, has improved significantly throughput and the level of automation of a whole set of production equipment; Two. can obtain in the production that granularity is large, the desirable boric acid crystallization of crystal formation, the constant product quality of boric acid is 99.9%; Three. greatly reduce energy consumption, to produce one ton of boric acid product, about power consumption is spent than ordinary process economize on electricity 100; Four. efficiently solve knot wall problem, crystal is difficult for being attached on the cooler wall, has fundamentally solved the low situation of rate of heat exchange, has also alleviated labour intensity; Five. we adopt the inflation method of negative pressure pressure will float crystalline substance and send into the secondary dissolving vessel, floating brilliant in the secondary dissolving vessel through heating the elimination degree of supersaturation, and then cooling, circulation, the crystallization of the system of participation material have so just effectively solved a floating brilliant difficult problem.
Technical scheme is: the technical process that the method for boric acid is produced in the continuous and automatic crystallization is the ore deposit acidifying of boron magnesium, filtering and impurity removing matter, crystallisation by cooling, remove by filter mother liquor, drying dewaters to such an extent that five operations of boric acid product are finished, it is characterized in that the crystallisation by cooling operation is split up into cooling, crystallization, negative pressure is taken away floating brilliant, adding four operations of water heating secondary dissolving finishes, the cooling temperature of refrigerating work procedure is 22-26 ℃, the negative pressure that negative pressure is taken away in the floating brilliant operation is 0.2-0.4 normal atmosphere, the Heating temperature that adds in the water heating secondary dissolution process is 70-80 ℃, the pH value that solution is regulated it with sulfuric acid is 2.95-3.05, adding solution after water heating secondary dissolution process is processed turns back in the refrigerating work procedure and recycles, have unnecessary feed liquid also to turn back in the refrigerating work procedure in the crystallization and recycle, the boric acid crystal that produces after the crystallization more after filtration, drying process just can obtain the boric acid product.The ore deposit acidifying of boron magnesium, filtering and impurity removing matter, crystallisation by cooling, remove by filter mother liquor, drying and dewater to such an extent that five operations of boric acid product are production technique of existing boric acid, it is prior art, here no longer describe in detail, existing crystallisation by cooling is that intermittent type is once finished, the present invention once finishes crystallisation by cooling with existing intermittent type to change continuous and automatic crystallization production into, thereby has overcome the deficiencies in the prior art.Refrigerating work procedure is the operation that feed liquid is cooled to suitable feed liquid Tc.Crystallization Procedure is the operation that feed liquid is produced the boric acid crystal, it is floating brilliant to produce some in this operation, these floating crystalline substances are taken floating brilliant operation away through negative pressure again and are pumped into to add in the water heating secondary dissolution process and process, adding water heating secondary dissolution process is front operation to be taken out the floating crystalline substance that comes add the water heating, regulate its pH value to the process of 2.95-3.05 with sulfuric acid again, add solution after water heating secondary dissolution process is processed and turn back in the refrigerating work procedure again and recycle, have unnecessary feed liquid also to turn back in the refrigerating work procedure in the crystallization and recycle.There is unnecessary feed liquid to refer to that this part feed liquid of not finishing crystallization in the crystallization time section of regulation is exactly unnecessary feed liquid in the crystallization, it can draw a circulating line in refrigerating work procedure by the certain altitude in crystallizer, and the feed liquid that exceeds is just guided in the refrigerating work procedure and can be realized by this circulating line.
Advantage of the present invention is: one. production technique has realized efficiently, the continuous and automatic crystallization, has improved significantly throughput and the level of automation of a whole set of production equipment; Two. material circulates in crystal system in the production, by controlling material flow velocity and crystallization time in cooling system well, and a plurality of factors such as cooling water flow, temperature of controlling just can obtain, and granularity is large, the desirable boric acid crystallization of crystal formation, and the constant product quality of boric acid is 99.9%; Three. greatly reduce energy consumption, to produce one ton of boric acid product, because this cover technique cooling efficiency is very high, power consumption can economize on electricity about 100 degree than ordinary process; Four. efficiently solve knot wall problem, the mode that adopts cooling and crystallization to separate is evenly cooled off material, the control material flow is in it and breathes heavily stream mode, and crystal just is difficult for being attached on the cooler wall like this, fundamentally solve the low situation of rate of heat exchange, also alleviated labour intensity; Five. effectively solve floating brilliant problem, floating brilliant small but can not grow up again, will have influence on the crystallisation process of boric acid, affect the service efficiency of crystallizer, continuous crystallisation also has floating brilliant the appearance in operational process, the floating crystal layer of the small entrained foam of particle is suspended in the top of crystallizer, we adopt the inflation method of negative pressure pressure will float crystalline substance and send into and add in the dissolving of water heating secondary, floating brilliant in adding the dissolving of water heating secondary through heating the elimination degree of supersaturation, and then the cooling of the system of participation material, the circulation of crystallization, so just effectively solve a floating brilliant difficult problem, improved the throughput of quality product and equipment.
Four, embodiment:
Embodiment 1: the method for boric acid is produced in the continuous and automatic crystallization, technical process is the ore deposit acidifying of boron magnesium, filtering and impurity removing matter, crystallisation by cooling, remove by filter mother liquor, drying dewaters to such an extent that five operations of boric acid product are finished, it is characterized in that the crystallisation by cooling operation is split up into cooling, crystallization, negative pressure is taken away floating brilliant, adding four operations of water heating secondary dissolving finishes, the cooling temperature of feed liquid is 22 ℃ in the refrigerating work procedure, the negative pressure that negative pressure is taken away in the floating brilliant operation is 0.2 normal atmosphere, the Heating temperature that adds in the water heating secondary dissolution process is 80 ℃, the pH value that solution is regulated it with sulfuric acid is 2.95, adding solution after water heating secondary dissolution process is processed turns back in the refrigerating work procedure and recycles, have unnecessary feed liquid also to turn back in the refrigerating work procedure in the crystallization and recycle, the boric acid crystal that produces after the crystallization more after filtration, drying process just can obtain the boric acid product.
Embodiment 2: the method for boric acid is produced in the continuous and automatic crystallization, technical process is the ore deposit acidifying of boron magnesium, filtering and impurity removing matter, crystallisation by cooling, remove by filter mother liquor, drying dewaters to such an extent that five operations of boric acid product are finished, it is characterized in that the crystallisation by cooling operation is split up into cooling, crystallization, negative pressure is taken away floating brilliant, adding four operations of water heating secondary dissolving finishes, the cooling temperature of feed liquid is 26 ℃ in the refrigerating work procedure, the negative pressure that negative pressure is taken away in the floating brilliant operation is 0.4 normal atmosphere, the Heating temperature that adds in the water heating secondary dissolution process is 70 ℃, the pH value that solution is regulated it with sulfuric acid is 3.05, adding solution after water heating secondary dissolution process is processed turns back in the refrigerating work procedure and recycles, have unnecessary feed liquid also to turn back in the refrigerating work procedure in the crystallization and recycle, the boric acid crystal that produces after the crystallization more after filtration, drying process just can obtain the boric acid product.
Embodiment 3: the method for boric acid is produced in the continuous and automatic crystallization, technical process is the ore deposit acidifying of boron magnesium, filtering and impurity removing matter, crystallisation by cooling, remove by filter mother liquor, drying dewaters to such an extent that five operations of boric acid product are finished, it is characterized in that the crystallisation by cooling operation is split up into cooling, crystallization, negative pressure is taken away floating brilliant, adding four operations of water heating secondary dissolving finishes, the cooling temperature of refrigerating work procedure feed liquid is 24 ℃, the negative pressure that negative pressure is taken away in the floating brilliant operation is 0.3 normal atmosphere, the Heating temperature that adds in the water heating secondary dissolution process is 75 ℃, the pH value that solution is regulated it with sulfuric acid is 3.00, adding solution after water heating secondary dissolution process is processed turns back in the refrigerating work procedure and recycles, unnecessary feed liquid also turns back in the refrigerating work procedure and recycles in the crystallization, and the boric acid crystal that produces after the crystallization more after filtration, drying process just can obtain the boric acid product.
Claims (1)
1. the method for boric acid is produced in a continuous and automatic crystallization, its technical process is the ore deposit acidifying of boron magnesium, filtering and impurity removing matter, crystallisation by cooling, remove by filter mother liquor, drying dewaters to such an extent that five operations of boric acid product are finished, it is characterized in that the crystallisation by cooling operation is split up into cooling, crystallization, negative pressure is taken away floating brilliant, adding four operations of water heating secondary dissolving finishes, the cooling temperature of refrigerating work procedure is 22-26 ℃, the negative pressure that negative pressure is taken away in the floating brilliant operation is 0.2-0.4 normal atmosphere, the Heating temperature that adds in the water heating secondary dissolution process is 70-80 ℃, the pH value that solution is regulated it with sulfuric acid is 2.95-3.05, adding solution after water heating secondary dissolution process is processed turns back in the refrigerating work procedure and recycles, have unnecessary feed liquid also to turn back in the refrigerating work procedure in the crystallization and recycle, the boric acid crystal that produces after the crystallization more after filtration, drying process just can obtain the boric acid product.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003375A (en) * | 2007-01-19 | 2007-07-25 | 段贵华 | Preparing boric acid by complete cycled recrystal method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003375A (en) * | 2007-01-19 | 2007-07-25 | 段贵华 | Preparing boric acid by complete cycled recrystal method |
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Application publication date: 20130327 |