CN104003451B - The preparation method of a kind of ferric chloride (FeCl36H2O) - Google Patents
The preparation method of a kind of ferric chloride (FeCl36H2O) Download PDFInfo
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- CN104003451B CN104003451B CN201410235109.3A CN201410235109A CN104003451B CN 104003451 B CN104003451 B CN 104003451B CN 201410235109 A CN201410235109 A CN 201410235109A CN 104003451 B CN104003451 B CN 104003451B
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Abstract
The present invention discloses the preparation method of a kind of ferric chloride (FeCl36H2O), it is characterised in that, comprise the following steps: first, it is determined that the reaction system preparing ferric chloride (FeCl36H2O) comprises H2O and FeCl3; Secondly, the batching coefficient ��=M_H of the reaction system of ferric chloride (FeCl36H2O) is prepared in setting2O/M_FeCl3, wherein M_H2O represents H2O in the total mass number of reaction system, M_FeCl3Represent FeCl3Total mass number in reaction system; Finally, according to batching coefficient ��=2/3, adjustment reaction system is H2O and FeCl3Total mass number, stir at 20 DEG C even leave standstill after 8 hours, stir to when starting to precipitate out solid, pour mould into, curing molding, obtain block ferric chloride (FeCl36H2O); Or, according to batching coefficient ��=0.89-1.2, adjustment reaction system is H2O and FeCl3Total mass number, stir cooling after, obtain sand-like ferric chloride (FeCl36H2O).
Description
Technical field
The present invention relates to the preparation method of a kind of ferric chloride (FeCl36H2O).
Background technology
Ferric chloride (FeCl36H2O) molecular formula: FeCl3.6H2O English name: Ferricchloridehexahydrate, outward appearance: isabelline crystal property: odorless, has astringent taste, water absorbability has by force deliquescence, can become reddish-brown liquid by deliquescence in atmosphere. Extremely soluble in water, the aqueous solution is strongly-acid, can make protein coagulating. It is soluble in ethanol, acetone, it is possible to be dissolved in sulfur dioxide liquid, ethamine, aniline, it is insoluble to glycerine, phosphorus trichloride. Purposes: be mainly used as water conditioner, the catalyzer of the etching reagent of plate making, electronic circuit chart board, the chlorizating agent of metallurgical industry, the oxygenant of dyestuffs industries and mordant, organic synthesis industry and oxygenant, chlorizating agent, be manufacture other molysite, pigment raw material and for mine ore dressing.
Traditional processing method can by FeCl3.6H2O makes sand-like, it is also possible to make irregular bulk. Its basic technique is: (1) is by FeCl3It is about 50% that solution is concentrated to mass concentration, and cooling and stirring goes out sand-like FeCl3.6H2O product; (2) by FeCl3Solution is concentrated to FeCl3Content is about 60%, allows its crystallisation by cooling become solid FeCl3.6H2O, then it is broken into irregular little bulk.
But, FeCl prepared by above-mentioned traditional processing method3.6H2O, its chemical purity is not good, foreign matter content height. In addition, irregular block FeCl is made3.6H2O, corner angle are too sharp, it is easy to puncture packing bag, enter moisture, cause FeCl3.6H2O is hydrolyzed and lumps, and not easily takes.
Summary of the invention
For above-mentioned technological deficiency, it is an object of the present invention to provide a kind of bulk or the preparation method of sand-like ferric chloride (FeCl36H2O), its FeCl3.6H2The purity height of O, product rate height, and technique is simple.
Another object of the present invention is to provide the preparation method of a kind of ferric chloride (FeCl36H2O), and its shape is half spherical, utilizes packaging and stores.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
(1) preparation method of a kind of ferric chloride (FeCl36H2O), it is characterised in that, comprise the following steps:
First, it is determined that the reaction system preparing ferric chloride (FeCl36H2O) comprises H2O and FeCl3;
Secondly, the batching coefficient ��=M_H of the reaction system of ferric chloride (FeCl36H2O) is prepared in setting2O/M_FeCl3, wherein M_H2O represents H2O in the total mass number of reaction system, M_FeCl3Represent FeCl3Total mass number in reaction system;
Finally, according to batching coefficient ��=2/3, adjustment reaction system is H2O and FeCl3Total mass number, stir at 20 DEG C even leave standstill after 8 hours, stir to when starting to precipitate out solid, pour mould into, curing molding, obtain block ferric chloride (FeCl36H2O).
Preferably, the reaction system of described ferric chloride (FeCl36H2O) also includes HCl and NaClO3��
Preferably, FeCl in described reaction system3For the FeCl of abstraction purification3; Its abstraction purification technique is: first by FeCl3It is dissolved in HCl and H2In O, by the organic solvent methyl-isobutyl-ketone in extraction tower or extracted with diethyl ether FeCl3, and then pass through H2O reextraction FeCl3Gained.
Preferably, according to batching coefficient ��=2/3, adjustment reaction system is H2O and FeCl3Total mass number, less than 20 DEG C stir even leave standstill after 8 hours, stir to, when starting to precipitate out solid, inserting less than 20 DEG C spontaneous curings in hemispherical, the demoulding after 2-3 hour also packs.
(2) preparation method of a kind of ferric chloride (FeCl36H2O), it is characterised in that, comprise the following steps:
First, it is determined that the reaction system preparing ferric chloride (FeCl36H2O) comprises H2O and FeCl3;
Secondly, the batching coefficient ��=M_H of the reaction system of ferric chloride (FeCl36H2O) is prepared in setting2O/M_FeCl3, wherein M_H2O represents H2O in the total mass number of reaction system, M_FeCl3Represent FeCl3Total mass number in reaction system;
Finally, according to batching coefficient ��=0.89-1.2, adjustment reaction system is H2O and FeCl3Total mass number, stir cooling after, obtain sand-like ferric chloride (FeCl36H2O).
Preferably, described choosing of batching coefficient �� increases with the rising of envrionment temperature.
Preferably, the reaction system of described ferric chloride (FeCl36H2O) also includes HCl and/or NaClO3��
Preferably, FeCl in described reaction system3For the FeCl of abstraction purification3; Its abstraction purification technique is: first by FeCl3It is dissolved in HCl and H2In O, by the organic solvent methyl-isobutyl-ketone in extraction tower or extracted with diethyl ether FeCl3, and then pass through H2O reextraction FeCl3Gained.
The present invention has creatively introduced the batching coefficient ��=M_H of the reaction system that is prepared ferric chloride (FeCl36H2O)2O/M_FeCl3, wherein=M_H2O represents H2O in the total mass number of reaction system, M_FeCl3Represent FeCl3Total mass number in reaction system; As long as measuring containing FeCl3Solution in FeCl3The percentage ratio of content (quality), so that it may obtain H best in reaction system2The percentage ratio of the quality of O.
Such as, FeCl is recorded3FeCl in solution3Content be 62%, namely 0.62, so H2The content of O is exactly 0.38, and namely 38%, it to be made FeCl3.6H2O, then should add H2O is set to X, (because FeCl3.6H2FeCl in O3Content theoretical value should be 60%, and namely 0.60, wherein ��=M_H2O/M_FeCl3Ratio be 2/3), be calculated as follows
��=M_H2O/M_FeCl3=(0.38+X)/0.62=2/3
Calculate X=0.0333, namely 3.33%, claim containing 62%FeCl3The weight of feed liquid be multiplied by 3.33%, be the quantity (total mass number) of the water that should add.
Otherwise, if FeCl3Content lower than 60%, then should add FERRIC CHLORIDE ANHYDROUS, and formula is as follows:
��=M_H2O/(M-FeCl3+ Y)=2/3
Such as, FeCl is recorded3Content is 58%, then should add FeCl3Quantity as follows:
��=0.42/ (0.58+Y)=2/3
Calculate Y=0.05, namely 5%. Claim containing 58%FeCl3The weight of feed liquid, then be multiplied by 5%, be the weight of the FERRIC CHLORIDE ANHYDROUS that should add.
According to above method, so that it may with will containing FeCl3The concentration of solution adjust to FeCl3Content is the concentration of 60%, i.e. FeCl3.6H2The content of O can reach 100%, and impurity also to be accounted for certain share, just H2The content of O is corresponding has lacked some.
At the sand-like FeCl of preparation3.6H2During O, the concept use of this �� value is bigger. According to envrionment temperature, it is possible to control between 0.89-1.20 by �� value, envrionment temperature is lower, and �� value should be bigger, because envrionment temperature is lower, and FeCl3Solubleness less, H2O deal has been lacked, precipitation too many, does not become sand-like crystal, becomes the colloid that mud is the same, do not dewater well, does not also have the effect of purifying. At the sand-like FeCl of preparation3.6H2During O, regulate �� value, then can greatly improve the quality of product, namely reach high-purity object.
The two of the contribution of the present invention are at the block FeCl of preparation3.6H2During O, it may also be useful to semicircle spherical mould. The FeCl prepared like this3.6H2O is half spherical, it does not have sharp corner angle, not easily puncture plastic packaging bag, ensure that sealing effect, can preserve for a long time, never degenerate. Another benefit is, half spherical has spherical face, and the face that contacts with each other is little, not easily adhesion; Especially during summer temperature height, even if there being an adhesion, also easily scattering, this is its another big advantage.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details.
Embodiment 1:
With FERRIC CHLORIDE ANHYDROUS (FeCl3) prepare sand-like ferric chloride (FeCl36H2O) (FeCl3.6H2O)
1000 liters of enamel glass jacket reaction narrow-necked earthen jars add pure water 700 liters, hydrochloric acid 15 liters, FERRIC CHLORIDE ANHYDROUS FeCl3800kg, filters with whizzer (canvas or 747 polypropylene fibre filter clothes) after stirring and dissolving; Vacuum filtration again (747 polypropylene fibre filter cloth), measures FeCl3Content.
According to envrionment temperature, it is determined that batching coefficient ��. Applicant is through a large amount of experimental verifications, and envrionment temperature 20 DEG C, 15 DEG C, 10 DEG C, 5 DEG C batching coefficient �� corresponding respectively are 0.9,1.0,1.1,1.2.
According to determining batching coefficient ��, calculate the add-on of pure water, it is ensured that �� value is transferred between 0.9-1.20, under agitation cools, allow it precipitate out FeCl3.6H2The sand-like crystallization of O.
Finally, whizzer dries, packaging. Packaging nexine is polyethylene food pack, and skin is the polyethylene bag of thickness 0.1mm, and outer is fiber can.
Embodiment 2:
Half spherical FeCl3.6H2O is prepared with anhydrous FeCl3
In 1000 liters of lass lining jacketed reaction narrow-necked earthen jars, add pure water 500 liters, hydrochloric acid 15 liters, anhydrous FeCl3FeCl is measured after 800kg stirring and dissolving2Content, then press FeCl2The mole number gradation of amount adds NaClO3(sodium chlorate), every 1 mole of FeCl2Gram NaClO that adds 17.67 altogether3. Application K3Fe(CN)6Inspection is without Fe+2Time, filter.
Filtrate is received in the plastic tank of 20 liters, every barrel of 20kg. Use SnCl2�CK2Cr2O7Method surveys FeCl3Percentage composition A, then add water adjustment by following formula
��=(1-A+x)/A=2/3
Obtain the mass percent that should add water, then it is multiplied by 20kg, be the water yield that should add. After adding water, stir even hold over night (less than 20 DEG C) after more than 8 hours, when stirring beginning crystallization, pour into as early as possible in dome-type mould, allow its spontaneous curing (less than 20 DEG C) be shaped; After 2-3 hour, the demoulding is poured out, and packs.
In addition, it is possible to use the sand-like FeCl that above embodiment 1 is made3.6H2O, after heat fused, is concentrated to ��=2/3 (i.e. FeCl3Content is 60%) time, make dome-type according to above step, content can reach more than 99%. Its foreign matter content is very low, because sand-like raw material is through purification.
Embodiment 3
Also can with the sand-like ferric chloride (FeCl36H2O) FeCl bought on the market3.6H2O carrys out purifying by above embodiment 1 or embodiment 2, manufactures sand-like FeCl3.6H2O or half spherical FeCl3.6H2O, when just calculating by �� value, will consider FeCl3.6H2The water (or also slightly some more) of existing 40% in O raw material, FeCl3Only accounted for for 60% (or also slightly lacking point).
Embodiment 4
Sand-like FeCl is prepared with reference to embodiment 13.6H2During O, it is also possible to use NaClO with reference to embodiment 23FeCl in oxidation removal solution2��
Embodiment 5
In order to obtain purer sand-like FeCl3.6H2O, it is possible to first with organic mixed solvent by FeCl3It is extracted in organic layer, then with isopyknic pure water by the FeCl in organic layer3In reextraction backwater. (choosing �� value according to envrionment temperature) by between aqueous phase evaporation concentration to ��=0.90-1.20, other steps are with embodiment 1.
Specifically, FeCl is extracted3Technique is: by 15kgFeCl3It is dissolved in 0.5 liter of HCl and 40 liter of H2In O. Agitation and filtration is (containing FeCl in this filtrate3It is about 37.5%) after, add 75 and rise HCl, be placed in the groove being equipped with recycle pump.
(1) by FeCl3It is extracted in organic phase, liter organic mixed solvent (methyl-isobutyl-ketone or ether) that adds 150 in extraction tower (being positioned on the top of recycle pump groove). ON cycle pump, allows FeCl3Solution undertaken extracting (1-5 time) by organic layer under upper pouring. Wait 15 minutes, allow two phase stratification. Lower floor's aqueous phase (about 115-120 liter) is released, forwards in waste liquid deposit groove, wait until him and use.
(2) by FeCl3Reextraction backwater phase again, then in recycle pump groove, add 150 liters of pure water, open extraction cycle pump, allow pure water under upper pouring, by organic layer, by FeCl3Reextraction backwater phase. , allow two-phase laminated flow 1-5 time repeatedly, then wait 15 minutes.
(3) taking out aqueous phase to forward in the concentrated narrow-necked earthen jar of reduction vaporization, concentrating under reduced pressure is to ��=0.9-1.20 (according to envrionment temperature), and cooling and stirring precipitates out sand-like FeCl3.6H2O��
Embodiment 6
In order to obtain the spherical FeCl of purer half3.6H2O, can by the obtained high-purity sand-like FeCl of embodiment 53.6H2After O heating for dissolving, add water according to ��=2/3 and regulate FeCl3Content is 60%, then makes half spherical FeCl by the step of embodiment 23.6H2O��
The present invention can improve FeCl3.6H2The product rate of O and purity; Other half spherical FeCl3.6H2O can prevent day thermal capacitance from easily luming, it may also be useful to convenient, and not easily punctures plastics bag, ensure that sealing effect, not easily the moisture absorption and lump.
Although embodiment of the present invention being described above, but the present invention is not limited to above-mentioned specific embodiments, above-mentioned specific embodiments is only schematic, guiding, instead of restrictive. The those of ordinary skill of this area is under the enlightenment of this specification sheets, and when not departing from the scope that the claims in the present invention are protected, it is also possible to make a variety of forms, these all belong to the row of the present invention's protection.
Claims (6)
1. the preparation method of a ferric chloride (FeCl36H2O), it is characterised in that, comprise the following steps:
First, it is determined that the reaction system preparing ferric chloride (FeCl36H2O) comprises H2O and FeCl3;
Secondly, the batching coefficient ��=M_H of the reaction system of ferric chloride (FeCl36H2O) is prepared in setting2O/M_FeCl3, wherein M_H2O represents H2O in the total mass number of reaction system, M_FeCl3Represent FeCl3Total mass number in reaction system;
Finally, according to batching coefficient ��=2/3, adjustment reaction system is H2O and FeCl3Total mass number, stir at 20 DEG C even leave standstill after 8 hours, stir to when starting to precipitate out solid, pour mould into, curing molding, obtain block ferric chloride (FeCl36H2O);
Wherein, the reaction system of described ferric chloride (FeCl36H2O) also includes HCl and NaClO3;
FeCl in described reaction system3For the FeCl of abstraction purification3; Its abstraction purification technique is: first by FeCl3It is dissolved in HCl and H2In O, by the organic solvent methyl-isobutyl-ketone in extraction tower or extracted with diethyl ether FeCl3, and then pass through H2O reextraction FeCl3Gained.
2. the preparation method of ferric chloride (FeCl36H2O) according to claim 1, it is characterised in that, according to batching coefficient ��=2/3, adjustment reaction system is H2O and FeCl3Total mass number, less than 20 DEG C stir even leave standstill after 8 hours, stir to, when starting to precipitate out solid, inserting less than 20 DEG C spontaneous curings in hemispherical, the demoulding after 2-3 hour also packs.
3. the preparation method of a ferric chloride (FeCl36H2O), it is characterised in that, comprise the following steps:
First, it is determined that the reaction system preparing ferric chloride (FeCl36H2O) comprises H2O and FeCl3;
Secondly, the batching coefficient ��=M_H of the reaction system of ferric chloride (FeCl36H2O) is prepared in setting2O/M_FeCl3, wherein M_H2O represents H2O in the total mass number of reaction system, M_FeCl3Represent FeCl3Total mass number in reaction system;
Finally, according to batching coefficient ��=0.89-1.2, adjustment reaction system is H2O and FeCl3Total mass number, stir cooling after, obtain sand-like ferric chloride (FeCl36H2O).
4. the preparation method of ferric chloride (FeCl36H2O) according to claim 3, it is characterised in that, described choosing of batching coefficient �� increases with the rising of envrionment temperature.
5. the preparation method of ferric chloride (FeCl36H2O) according to claim 3, it is characterised in that, the reaction system of described ferric chloride (FeCl36H2O) also includes HCl and/or NaClO3��
6. the preparation method of ferric chloride (FeCl36H2O) according to claim 3, it is characterised in that, FeCl in described reaction system3For the FeCl of abstraction purification3; Its abstraction purification technique is: first by FeCl3It is dissolved in HCl and H2In O, by the organic solvent methyl-isobutyl-ketone in extraction tower or extracted with diethyl ether FeCl3, and then pass through H2O reextraction FeCl3Gained.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85108552A (en) * | 1985-11-27 | 1987-06-03 | 北京大学 | The treatment process of chlorhydric acid pickling waste containing iron |
| CN1673415A (en) * | 2004-03-23 | 2005-09-28 | 上海奉贤四团化工试剂厂 | Separation of nickel ion in iron trichloride solution by crystallization and extraction method |
| CN102701290A (en) * | 2012-06-19 | 2012-10-03 | 惠州市斯瑞尔环境化工有限公司 | Method for preparing blocky ferric trichloride |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85108552A (en) * | 1985-11-27 | 1987-06-03 | 北京大学 | The treatment process of chlorhydric acid pickling waste containing iron |
| CN1673415A (en) * | 2004-03-23 | 2005-09-28 | 上海奉贤四团化工试剂厂 | Separation of nickel ion in iron trichloride solution by crystallization and extraction method |
| CN102701290A (en) * | 2012-06-19 | 2012-10-03 | 惠州市斯瑞尔环境化工有限公司 | Method for preparing blocky ferric trichloride |
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