CN104961160A - Production method for granular anhydrous manganese chloride - Google Patents
Production method for granular anhydrous manganese chloride Download PDFInfo
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Abstract
The invention provides a production method for granular anhydrous manganese chloride. The production method includes the steps that a manganese chloride concentrated solution with the concentration of 45-52 baume degrees is obtained through raw material reaction, impurity removal, filtration and concentration and sprayed into a drying granulator at the set temperature to be dried and granulated; anhydrous manganese chloride granules are screened after granulation, and the large anhydrous manganese chloride granules obtained after screening are fed into a disc vacuum dryer at constant speed to be dried in a vacuum mode; the anhydrous manganese chloride granules are cooled in a vacuum partition mode and packaged in a sealed mode. According to the granulating and drying method, the drying granulator is heated, then a small amount of manganese chloride concentrated solution is added into the drying granulator, after tiny manganese chloride crystals are formed, the manganese chloride concentrated solution is sprayed into the drying granulator, and under the action of kneading and stirring, the manganese chloride crystals grow up into the compact manganese chloride granules to form new tiny manganese chloride crystals. The production method has the advantages of being simple in technology, convenient to operate, environmentally friendly, stable in production quality, high in activity and long in shelf life and saving energy.
Description
Technical field
The invention belongs to inorganic chemical product production field, particularly relate to production method and the drying-granulating method and apparatus of particulate state Manganese chloride anhydrous.
Background technology
Manganese chloride anhydrous has a wide range of applications in the field such as medicine synthesis, feed auxiliary, analytical reagent, pigment manufacture, alloy smelting, drying battery manufacture.Granular anhydrous Manganous chloride tetrahydrate does not produce airborne dust when using, and can meet the demand that people improve Working environment and Occupational health, can also reduce material loss; Meanwhile, the proportion of granular anhydrous Manganous chloride tetrahydrate is larger than powdered anhydrous Manganous chloride tetrahydrate, can reduce packaging, transport, carrying cost.Activity is high, water content is low, moisture content is evenly the expectation of Manganese chloride anhydrous client to its quality.The Product Activity of Manganese chloride anhydrous and the moisture content stability influence to the making formula of its derived product and performance is comparatively large, therefore exploitation active high, moisture content is low and evenly, quality guarantee period long anhydrous granular Manganous chloride tetrahydrate be the inexorable trend improving the enterprise product market competitiveness.
At present, the production drying process of granular anhydrous Manganous chloride tetrahydrate mainly contains two kinds: one is static pellet type desiccating method, the method labor strength is large, the easy efflorescence of product granular loose, material does not flow, doing of product is wet lack of homogeneity and easily occurs that the use of the overbaking phenomena impair products such as stain macula lutea is active, and the initial moisture of finished product is generally more than 0.5%.Another kind is fluidized bed prilling oven drying method, and during oven dry, air quantity is large, and the amount that tiny Manganese chloride anhydrous enters scrubber tower is just many, affects the oven dry energy consumption of Manganese chloride anhydrous; Air quantity is large, vacuum-drying can not be carried out, drying temperature is high, need use the blackening flavescence phenomenon that stronger acidic conditions causes to weaken high temperature and oxygen Manganese chloride anhydrous, and the surface irregularity after formed product, granular texture are loose, low, the easy secondary efflorescence of proportion and the moisture absorption.Hyperthermia drying and stronger acidity, large to equipment corrosion, control there is disadvantageous effect to the purity of product and production cost, in addition, hyperthermia drying and stronger acidity are also unfavorable for the health of environment protection and field personnel.
Summary of the invention
For prior art above shortcomings, the object of the present invention is to provide that a kind of technique is simple, easy to operate, energy-conserving and environment-protective and constant product quality, active high, granular anhydrous Manganous chloride tetrahydrate that quality guarantee period is long production method.
To achieve these goals, the technical solution used in the present invention is as follows: a kind of production method of granular anhydrous Manganous chloride tetrahydrate, is characterized in that, comprise the steps:
1) material: manganese metal or manganese salt and hydrochloric acid are reacted according to the mol ratio of 1:1.96-2.01, the pH value controlling material terminal is 4.3-6.5, and generation concentration is 34-38
othe manganese chloride solution of B é;
2) removal of impurities: in whipping process, slowly adds cleaner in above-mentioned material liquid, removing impurity, and temperature of reaction controls at 60-100 DEG C; Stirring reaction 2-3 hour, adds pH adjusting agent to regulate the pH value of manganese chloride solution, when the pH value of manganese chloride solution is stabilized in 5-7, filters and obtains Manganous chloride tetrahydrate except mixture solution;
3) filter: first will through step 2) filtering except mixture solution pressure filter after process, obtain Manganous chloride tetrahydrate just filtrate and residue, again first for Manganous chloride tetrahydrate filtrate is filtered through accurate filter, then add hydrochloric acid and regulate pH value, obtain the Manganous chloride tetrahydrate essence filtrate that pH value is stabilized in 3.8-6;
4) concentrated: by Manganous chloride tetrahydrate essence filtrate simmer down to concentration 45-52
othe Manganous chloride tetrahydrate concentrated solution of B é;
5) granulating and drying: at a set temperature, sprays into manganese chloride solution in drying-granulating machine, carries out granulating and drying;
6) sieve: granulation post chlorization manganese particle is crossed 16 mesh sieves, the Manganous chloride tetrahydrate particle under sieve returns in the smart filtrate of step 3), and the Manganous chloride tetrahydrate particle on sieve proceeds in feed bin;
7) vacuum-drying: by step 6) sieve on Manganous chloride tetrahydrate particle at the uniform velocity feeding in disc type Vacuumdrier, at 200-210 DEG C, carry out vacuum-drying 2.5-3.5 hour;
8) cool, pack: dried Manganous chloride tetrahydrate particle is placed and carries out dividing wall type cooling under vacuum conditions, be cooled to pack during 60-73 DEG C.
Wherein, step 2) described in cleaner can adopt mass concentration is the hydrogen peroxide solution of 10%-27.5%, freshly prepared mass concentration is 3%-26% barium carbonate slurry, mass concentration is one or more in the barium chloride solution of 20%.
Wherein, step 5) comprises the following steps:
(1) first will be heated to 155 DEG C-200 DEG C in granulating and drying machine, then add a small amount of Manganous chloride tetrahydrate concentrated solution, make it the fine crystalline body becoming Manganous chloride tetrahydrate;
(2) when reaching design temperature 155-200 DEG C, Manganous chloride tetrahydrate concentrated solution is pressed 0.12-0.20m with droplet-like
3the speed of/h is sprayed on the fine crystalline body of the Manganous chloride tetrahydrate in granulating and drying machine, carries out quick dewatering drying;
(3) under the kneading and tipping effect of granulating and drying machine, the pore formed during Manganous chloride tetrahydrate concentrated solution drying and dehydrating is eliminated rapidly, Manganous chloride tetrahydrate xln is grown up gradually and is formed fine and close Manganous chloride tetrahydrate particle, meanwhile, forms the fine crystalline body of new Manganous chloride tetrahydrate.
The particle diameter of the Manganous chloride tetrahydrate particle under the sieve described in step 6) is less than 1mm.
Main points one of the present invention are, control the size of granulation product by controlling the measures such as input concentration, spray flow, drying temperature, kneading intensity, obtain the large proportion granular particle that fine and close circle is real simultaneously.By adopting thermal oil to be that thermal source carries out dividing wall type heating, first the interlayer thermal oil of granulating and drying machine is warming up to 155 DEG C-200 DEG C, a little material is added again in granulating and drying machine, be dried to temperature of charge when reaching more than 90 DEG C, Manganous chloride tetrahydrate height solution is sprayed at droplet-like on the high-temp chlorination manganese fine particle in granulating and drying machine, carries out quick dewatering drying; Simultaneously material in granulating and drying machine by ceaselessly kneading with stir, the pore formed when product drying is dewatered can be eliminated rapidly, Manganous chloride tetrahydrate is spread upon Manganous chloride tetrahydrate particle exterior by layer upon layer even compact and grows up gradually like this, does not stop to form new particle centre simultaneously.
Main points two of the present invention are, the stoving process of Manganese chloride anhydrous gets up by Flow of Goods and Materials, obtain vacuum-drying and the cooling technology of uniformly transfer heat; Ambient moisture when reducing the drying temperature of Manganese chloride anhydrous, cooling and cooling time, thus the oxygen reduced in Manganese chloride anhydrous and air and contact with moisture and the possibility of deterioration by oxidation, the moisture absorption occurs.When the product granularity of materials inside granulating drier reaches 1-5 millimeter, open granulating and drying machine discharge port, material is slowly proceeded to vibratory screening apparatus, after crossing 16 mesh sieve screenings, the particle of < 1 millimeter is returned leading portion and promote strength of solution.Screen overflow is sent in feed bin, carries out at the uniform velocity feed and sends in disc type Vacuumdrier and carry out packaging after drying, cooling.
In addition, the manganese chloride solution in the present invention also can be able to be removal of impurities again after other manganese reactant salts such as hydrochloric acid and manganous carbonate by manganese sheet and hydrochloric acid reaction, filtration, purification and obtaining.Concrete dedoping step selects different impurity-removing methods and different cleaners, oxygenant, precipitation agent and sorbent material according to the impurity situation in solution.Wherein, impurity removing technology adopts existing technology.Solid load after press filtration is very low, negligible.The foreign matter content of Manganous chloride tetrahydrate product and purity can meet the industry standard of Manganous chloride tetrahydrate.
Practice shows, the water vapour produced when Manganous chloride tetrahydrate is dry under vacuum conditions in the present invention can be taken away rapidly, rate of drying is enhanced about more than once than traditional drying mode, and drying residencing time reduces by more than 50, and reduces active after can effectively avoiding it that oxidation flavescence blackening occurs.Carry out dividing wall type cooling under vacuum state, can avoid the product moisture absorption and cooling thoroughly and the packaging caused scorches situation and occurs, initial moisture can be low to moderate within 0.15%.This invention can reach more than 1.8 grams per milliliters with the Manganous chloride tetrahydrate pellet density that dry kneading on one side is on one side obtained, and product circle is real fine and close, and moisture absorption speed is 1/3rd under other drying processes; Granular anhydrous Manganous chloride tetrahydrate is according to the packing instructions of common product, and its moisture can long-term stability maintain within 0.5%, and quality guarantee period can reach more than 6 months.
Compared to existing technology, the present invention has following beneficial effect:
1, the production method of granular anhydrous Manganous chloride tetrahydrate provided by the invention is adopted, produce without secondary dust, material loss is little, can control the size of granulation product by controlling the measures such as input concentration, spray flow, drying temperature and kneading intensity, the Manganous chloride tetrahydrate particle of gained is solid, without the need to carrying out whole grain process, smooth surface, can not produce secondary efflorescence, fine and close particle surface structure densification, like having wrapped the moistureproof clothing of one deck to Manganous chloride tetrahydrate, substantially increases the anti-moisture absorption of product.By the Manganese chloride anhydrous of identical weight under different process state, expose in the environment of relative humidity 75% simultaneously, place 10 hours, the weightening finish of the Manganese chloride anhydrous under this technique only has 1/3rd under other techniques.
2, the granular anhydrous Manganous chloride tetrahydrate that the production method manufacture provided is provided is adopted, under vacuum, the aqueous vapor produced when Manganous chloride tetrahydrate is dry, can be taken away fast, avoid the Manganese chloride anhydrous that first generates by the moisture absorption repeatedly, repeatedly dry, and the bivalent manganese oxidation caused generates the value Mn such as trimanganese tetroxide or Manganse Dioxide, causes the water-insoluble of Manganous chloride tetrahydrate to raise, thus reduce the activity of Manganese chloride anhydrous, affect using and filling a prescription of client.
3, adopt the granular anhydrous Manganous chloride tetrahydrate production method that provides is provided and manufactured, both overcome static dry time, material dry wet irregular, returns artificial, energy dissipation when drying dry; When overcoming again boiled bed drying, bake out temperature is high, and heat energy loss is large, the easy oxidized rotten shortcoming of bivalent manganese.Vacuum-drying reduces the drying temperature of material, and improve the rate of drying more than one times of material, residence time of material only has 2.5-3.5 hour, and the activity of product is ensured further.
4, adopt the granular anhydrous Manganous chloride tetrahydrate inventing the production method manufacture provided, the later stage carries out cooling rear packaging under vacuum conditions, for the quality guarantee extending product is given security.Temperature of charge uniform, controllable after dynamic cooling under vacuum, can avoid the moisture absorption again of product under the general type of cooling; Under can also avoiding the general type of cooling, material cooling temperature height differs simultaneously, causes local temperature too high and scorches packing bag and cause the product moisture absorption.
5, adopt the granular anhydrous Manganous chloride tetrahydrate compact structure inventing the production method manufacture provided, the initial uniform moisture of product, and can be low to moderate less than 0.15%, the moisture absorption of product is well below the Manganese chloride anhydrous finished product obtained by other production technique.Its quality guarantee period can reach more than 6 months, than the granular anhydrous Manganous chloride tetrahydrate length more than 3 months of existing explained hereafter.
6, in process of production, especially avoid in a step granulation, vacuum-drying, vacuum cooling and wrapping process compared with the granulation under strong acidic condition and oven dry, decrease the corrosion to equipment and the secondary pollution to product.Adopt the granular anhydrous Manganous chloride tetrahydrate of this Technology manufacture both to save the energy, reduce the corrosion to equipment, protect environment again, be more conducive to the occupational health protection of field personnel.
Accompanying drawing explanation
Fig. 1 is method steps schema of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
embodiment 1:a production method for granular anhydrous Manganous chloride tetrahydrate, comprises the steps:
1) material: manganous carbonate and hydrochloric acid are reacted according to the mol ratio of 1:1.96, obtaining concentration is 38
othe manganese chloride solution of B é; The pH value controlling material terminal is 6.5;
2) removal of impurities: in whipping process, in above-mentioned material liquid, slowly add the barium chloride solution etc. that concentration is 27.5% hydrogen peroxide and concentration 20%, temperature of reaction controls at 60 DEG C; Stirring reaction 3.0 hours, adds pH adjusting agent to regulate the pH value of manganese chloride solution, when the pH value of manganese chloride solution is stabilized in 6.0, filters and obtains Manganous chloride tetrahydrate except mixture solution.
3) filter: cross and filter insolubles, obtain Manganous chloride tetrahydrate refined soln after essence filter, regulator solution PH is 4.5.
4) concentrated: Manganous chloride tetrahydrate refined soln to be carried out multiple-effect vacuum and is evaporated to 52
ob é, time condensation water returns material system material after entering and absorbing washing tower.
5) granulating and drying: by 52
owith 0.12m under the manganese chloride solution insulation of B é
3/ h pumps in drying-granulating machine, controls drying temperature 155 DEG C and carries out drying-granulating.
6) sieve: material is slowly proceeded to vibratory screening apparatus, cross 16 mesh sieves, the Manganous chloride tetrahydrate particle under sieve returns in the smart filtrate of step (3), and the Manganous chloride tetrahydrate particle on sieve proceeds in feed bin;
7) vacuum-drying: particle of being got the raw materials ready by pink Manganous chloride tetrahydrate proceeds in feed bin, more at the uniform velocity feed to send in disc type Vacuumdrier at 200 DEG C dry 2 hours 30 minutes.
8) cool, packaging: dried Manganous chloride tetrahydrate particle is placed and carries out dividing wall type cooling under vacuum conditions, switch after will being cooled to 68 DEG C and enter A, B two Material collecting box for harvesting and to gather materials in turn and blowing is packed in turn.
The granular anhydrous Manganous chloride tetrahydrate product that the method obtains, its outward appearance is the real spheroidal particle of smooth circle, with uniform lightpink, without stain, without macula lutea, active high.Its initial water is divided into 0.079%, and in Manganese chloride anhydrous particle, particle diameter is 4.5 millimeters.Through the tracking test of 6 months, the moisture of product was 0.38%; Through the tracking test of 9 months, the moisture of product was 0.45%.
embodiment 2:a production method for granular anhydrous Manganous chloride tetrahydrate, comprises the steps:
1) material: manganous carbonate and hydrochloric acid are reacted according to the mol ratio of 1:1.98, obtaining concentration is 36
oBthe manganese chloride solution of é, the pH value controlling material terminal is 5.6.
2) removal of impurities: in whipping process, in above-mentioned material liquid, slowly add concentration is the hydrogen peroxide of 15% and the barium carbonate slurry of fresh synthesis (containing barium carbonate about 26%), temperature of reaction controls at 75 DEG C, stirring reaction 2.5 hours, add pH adjusting agent to regulate the pH value of manganese chloride solution, when the pH value of manganese chloride solution is stabilized in 6.5, filters and obtain Manganous chloride tetrahydrate except mixture solution.
3) filter: cross and filter insolubles, obtain Manganous chloride tetrahydrate refined soln after essence filter, regulator solution PH is 5.
4) concentrated: Manganous chloride tetrahydrate refined soln to be carried out multiple-effect vacuum and is evaporated to 50
oBé, time condensation water returns material system material after entering and absorbing washing tower.
5) granulating and drying: by 50
oBwith 0.15m under the manganese chloride solution insulation of é
3/ h pumps in drying-granulating machine, controls drying temperature 175 DEG C and carries out drying-granulating.
6) sieve: carry out a sieving separating, cross 16 mesh sieves, the Manganous chloride tetrahydrate particle under sieve returns in the smart filtrate of step (3), and the Manganous chloride tetrahydrate particle on sieve proceeds in feed bin;
7) vacuum-drying: particle of being got the raw materials ready by pink Manganous chloride tetrahydrate proceeds in feed bin, more at the uniform velocity feed to send in disc type Vacuumdrier at 205 DEG C dry 2 hours 50 minutes;
8) cool, packaging: dried Manganous chloride tetrahydrate particle is carried out dividing wall type cooling under vacuum conditions, after Manganous chloride tetrahydrate particle is cooled to 73 DEG C switch enter A, B two Material collecting box for harvesting gather materials in turn and in turn blowing packaging.
The granular anhydrous Manganous chloride tetrahydrate product of gained, its outward appearance is the real spheroidal particle of smooth circle, with uniform lightpink, without stain, without macula lutea, active high.Its initial water is divided into 0.089%, and in Manganese chloride anhydrous particle, particle diameter is 3.8 millimeters.Through the tracking test of 6 months, the moisture of product was 0.36%; Through the tracking test of 9 months, the moisture of product was 0.43%.
embodiment 3:a production method for granular anhydrous Manganous chloride tetrahydrate, comprises the steps:
1) material: manganese sheet and hydrochloric acid are reacted according to the mol ratio of 1:1.99, obtaining concentration is 36
oBthe manganese chloride solution of é, the pH value controlling material terminal is 5.0.
2) removal of impurities: in whipping process, in above-mentioned material liquid, slowly add concentration is the hydrogen peroxide of 10% and the barium carbonate slurry of fresh synthesis (containing barium carbonate about 3%), and temperature of reaction controls at 86 DEG C; Stirring reaction 2 hours 40 points, adds pH adjusting agent to regulate the pH value of manganese chloride solution, when the pH value of manganese chloride solution is stabilized in 5.5, filters and obtains Manganous chloride tetrahydrate except mixture solution.
3) filter: cross and filter insolubles, obtain Manganous chloride tetrahydrate refined soln after essence filter, regulator solution PH is 6.
4) concentrated: Manganous chloride tetrahydrate refined soln to be carried out multiple-effect vacuum and is evaporated to 48
oBé, time condensation water returns material system material after entering and absorbing washing tower.
5) granulating and drying: by 48
oBwith 0.18m under the manganese chloride solution insulation of é
3/ h pumps in drying-granulating machine, controls drying temperature 185 DEG C and carries out drying-granulating.
6) sieve: carry out sieving separating, cross 16 mesh sieves, the Manganous chloride tetrahydrate particle under sieve returns in the smart filtrate of step (3), and the Manganous chloride tetrahydrate particle on sieve proceeds in feed bin;
7) vacuum-drying: particle of being got the raw materials ready by pink Manganous chloride tetrahydrate proceeds in feed bin, more at the uniform velocity feed to send in disc type Vacuumdrier at 203 DEG C dry 3 hours 10 minutes;
8) cool, packaging: after partition is cooled to 65 DEG C, switch enter A, B two Material collecting box for harvesting gather materials in turn and in turn blowing packaging.
The outward appearance of gained granular anhydrous Manganous chloride tetrahydrate product is the real spheroidal particle of smooth circle, with uniform lightpink, without stain, without macula lutea, active high.Its initial water is divided into 0.091%, and in Manganese chloride anhydrous particle, particle diameter is 3.0 millimeters.Through the tracking test of 6 months, the moisture of product was 0.37%; Through the tracking test of 9 months, the moisture of product was 0.45%.
embodiment 4:a production method for granular anhydrous Manganous chloride tetrahydrate, comprises the steps:
1) material: manganese sheet and hydrochloric acid are reacted according to the mol ratio of 1:2.01, obtaining concentration is 34
oBthe manganese chloride solution of é, the pH value controlling material terminal is 4.3.
2) removal of impurities: in whipping process, in above-mentioned material liquid, slowly add the hydrogen peroxide that concentration is 10%, temperature of reaction controls at 100 DEG C; Stirring reaction 2 hours, adds pH adjusting agent to regulate the pH value of manganese chloride solution, when the pH value of manganese chloride solution is stabilized in 5.2, filters and obtains Manganous chloride tetrahydrate except mixture solution.
3) filter: cross and filter insolubles, obtain Manganous chloride tetrahydrate refined soln after essence filter, regulator solution PH is 3.8.
4) concentrated: Manganous chloride tetrahydrate refined soln to be carried out multiple-effect vacuum and is evaporated to 45
oBé, time condensation water returns material system material after entering and absorbing washing tower.
5) granulating and drying: by 45
oBwith 0.20m under the manganese chloride solution insulation of é
3/ h pumps in drying-granulating machine, controls drying temperature 200 DEG C and carries out drying-granulating, sieves to obtain pink Manganous chloride tetrahydrate and to get the raw materials ready particle.
6) sieve: carry out sieving separating, cross 16 mesh sieves, the Manganous chloride tetrahydrate particle under sieve returns in the smart filtrate of step (3), and the Manganous chloride tetrahydrate particle on sieve proceeds in feed bin;
7) vacuum-drying: particle of being got the raw materials ready by pink Manganous chloride tetrahydrate proceeds in feed bin, carries out at the uniform velocity feed and to send in disc type Vacuumdrier at 210 DEG C dry 3 hours 30 minutes;
8) cool, packaging: then partition is cooled to 60 DEG C, switch enter A, B two Material collecting box for harvesting gather materials in turn and in turn blowing packaging.
The outward appearance of gained granular anhydrous Manganous chloride tetrahydrate product is the real spheroidal particle of smooth circle, with uniform lightpink, without stain, without macula lutea, active high.Its initial water is divided into 0.088%, in Manganese chloride anhydrous particle, particle diameter is 1.5 millimeters.Through the tracking test of 6 months, the moisture of product was 0.32%; Through the tracking test of 9 months, the moisture of product was 0.48%.
To sum up, the quality of Manganous chloride tetrahydrate particle that above-described embodiment obtains refers to following table:
| Initial moisture, % | Particle diameter, mm | Moisture after 6 months, % | Moisture after 9 months, % | |
| Embodiment 1 | 0.079 | 4.5 | 0.38 | 0.45 |
| Embodiment 2 | 0.089 | 3.8 | 0.36 | 0.43 |
| Embodiment 3 | 0.091 | 3 | 0.37 | 0.45 |
| Embodiment 4 | 0.088 | 1.5 | 0.32 | 0.48 |
In the present invention, effectively can control the particle diameter of granulation product by controlling the measures such as input concentration, spray flow, drying temperature, kneading intensity, obtaining fine and close round real, heavy granular product.Wherein, the drying-granulating machine of use, its hot spots is designed to recuperative heat exchanger.The heat-conducting medium of described recuperative heat exchanger is thermal oil.
Showing through practice, by adjusting the parameter such as flow of the concentration of solution, bake out temperature, solution, the Manganese chloride anhydrous of different average particle size can be obtained.Usually, the concentration of solution is higher, and the prilling temperature of needs is lower, and flow is less, and the particle diameter of the granular anhydrous Manganous chloride tetrahydrate of gained is larger; Otherwise the particle diameter of the granular anhydrous Manganous chloride tetrahydrate of gained is less.Due to this granulation process carry out be drying and dehydrating while carry out granulating and forming, the particle Manganese chloride anhydrous of gained, compact structure, smooth surface, can not produce secondary dust, and the humidity resistance of product improves; In addition, after adopting vacuum decompression dynamic drying, then to carry out under vacuum state packaging after partition cooling, product-free overbaking low under guaranteeing the drying and packaging technique that the initial water proportion by subtraction of product is general, can be low to moderate within 0.15%.Both organically combines the production carrying out granular anhydrous Manganous chloride tetrahydrate, produce without dust and objectionable impurities, safety, energy-conserving and environment-protective can be met and guarantee the requirement of workman's Occupational health, fully can meet downstream client to product low moisture, high reactivity, long quality guaranteed period, the demand that produces without secondary dust.During vacuum-drying, water vapour can be taken away rapidly, reduces active after can effectively avoiding it that oxidation blackening flavescence occurs.Dividing wall type cooling is carried out under vacuum state, the product moisture absorption and cooling can be avoided not thoroughly and the packaging caused scorches situation and occurs, initial moisture can be low to moderate less than 0.1%, kneading while drying under the present invention, the Manganous chloride tetrahydrate pellet density that can obtain reaches more than 1.8 grams per milliliters, and product circle is real fine and close, and granular anhydrous Manganous chloride tetrahydrate is according to the packing instructions of common product, its moisture can long-term stability maintain within 0.5%, and quality guarantee period can reach 9 months.
The above embodiment of the present invention is only for example of the present invention is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (3)
1. a production method for granular anhydrous Manganous chloride tetrahydrate, is characterized in that, comprises the steps:
1) material: manganese metal or manganese salt and hydrochloric acid are reacted according to the mol ratio of 1:1.96-2.01, the pH value controlling material terminal is 4.3-6.5, and generation concentration is 34-38
othe manganese chloride solution of B é;
2) removal of impurities: in whipping process, in above-mentioned material liquid, slowly add cleaner, temperature of reaction controls at 60-100 DEG C; Stirring reaction 2-3 hour, adds pH adjusting agent to regulate the pH value of manganese chloride solution, when the pH value of manganese chloride solution is stabilized in 5.2-6.5, filters and obtains Manganous chloride tetrahydrate except mixture solution;
3) filter: first will through step 2) filtering except mixture solution pressure filter after process, obtain Manganous chloride tetrahydrate just filtrate and residue, again first for Manganous chloride tetrahydrate filtrate is filtered through accurate filter, then add hydrochloric acid and regulate pH value, obtain the Manganous chloride tetrahydrate essence filtrate that pH value is stabilized in 3.8-6.0;
4) concentrated: by Manganous chloride tetrahydrate essence filtrate simmer down to concentration 45-52
othe Manganous chloride tetrahydrate concentrated solution of B é;
5) granulating and drying: at a set temperature, sprays into manganese chloride solution in drying-granulating machine, carries out granulating and drying;
6) sieve: granulation post chlorization manganese particle is crossed 16 mesh sieves, the Manganous chloride tetrahydrate particle under sieve returns in the smart filtrate of step 3), and the Manganous chloride tetrahydrate particle on sieve proceeds in feed bin;
7) vacuum-drying: by step 6) sieve on Manganous chloride tetrahydrate particle at the uniform velocity feeding in disc type Vacuumdrier, at 200-210 DEG C, carry out vacuum-drying 2.5-3.5 hour;
8) cool, pack: dried Manganous chloride tetrahydrate particle is placed and carries out dividing wall type cooling under vacuum conditions, be cooled to pack during 60-73 DEG C.
2. the production method of particulate state Manganese chloride anhydrous according to claim 1, it is characterized in that, step 5) comprises the following steps:
(1) first will be heated to 155 DEG C-200 DEG C in granulating and drying machine, then add a small amount of Manganous chloride tetrahydrate concentrated solution, make it the fine crystalline body becoming Manganous chloride tetrahydrate;
(2) when reaching design temperature 155-200 DEG C, Manganous chloride tetrahydrate concentrated solution is pressed 0.12-0.20m with droplet-like
3the speed of/h is sprayed on the fine crystalline body of the Manganous chloride tetrahydrate in granulating and drying machine, carries out quick dewatering drying;
(3) under the kneading and tipping effect of granulating and drying machine, the pore formed during Manganous chloride tetrahydrate concentrated solution drying and dehydrating is eliminated rapidly, Manganous chloride tetrahydrate xln is grown up gradually and is formed fine and close Manganous chloride tetrahydrate particle, meanwhile, forms the fine crystalline body of new Manganous chloride tetrahydrate.
3. the production method of granular anhydrous Manganous chloride tetrahydrate according to claim 1, it is characterized in that, the particle diameter of the Manganous chloride tetrahydrate particle under the sieve described in step 6) is less than 1mm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5626722A (en) * | 1979-08-07 | 1981-03-14 | Nippon Steel Corp | Manufacture of manganese chloride |
| RU2179529C1 (en) * | 2000-07-07 | 2002-02-20 | Институт органического синтеза Уральского отделения Российской академии наук | Method of preparing anhydrous manganese chloride |
| CN102115197A (en) * | 2010-12-31 | 2011-07-06 | 谢善情 | Method for preparing manganese chloride and ferrous chloride by using manganese tailings |
| CN102674465A (en) * | 2012-05-23 | 2012-09-19 | 贵州红星发展股份有限公司 | Method for recycling chlorine gas from HCl-containing exhaust gas and preparing manganese chloride, and manganese chloride crystals |
| CN104310487A (en) * | 2014-09-30 | 2015-01-28 | 江西西林科股份有限公司 | Method for preparing anhydrous manganese chloride under anhydrous reaction conditions |
-
2015
- 2015-06-26 CN CN201510360850.7A patent/CN104961160B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5626722A (en) * | 1979-08-07 | 1981-03-14 | Nippon Steel Corp | Manufacture of manganese chloride |
| RU2179529C1 (en) * | 2000-07-07 | 2002-02-20 | Институт органического синтеза Уральского отделения Российской академии наук | Method of preparing anhydrous manganese chloride |
| CN102115197A (en) * | 2010-12-31 | 2011-07-06 | 谢善情 | Method for preparing manganese chloride and ferrous chloride by using manganese tailings |
| CN102674465A (en) * | 2012-05-23 | 2012-09-19 | 贵州红星发展股份有限公司 | Method for recycling chlorine gas from HCl-containing exhaust gas and preparing manganese chloride, and manganese chloride crystals |
| CN104310487A (en) * | 2014-09-30 | 2015-01-28 | 江西西林科股份有限公司 | Method for preparing anhydrous manganese chloride under anhydrous reaction conditions |
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| CN104961160B (en) | 2016-08-24 |
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