CN103466707A - Production method of chromic chloride hexahydrate - Google Patents
Production method of chromic chloride hexahydrate Download PDFInfo
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- CN103466707A CN103466707A CN2013103746974A CN201310374697A CN103466707A CN 103466707 A CN103466707 A CN 103466707A CN 2013103746974 A CN2013103746974 A CN 2013103746974A CN 201310374697 A CN201310374697 A CN 201310374697A CN 103466707 A CN103466707 A CN 103466707A
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Abstract
The invention discloses a production method of chromic chloride hexahydrate, which comprises the following steps that chromic anhydride is added to a reaction vessel; water with 60-80% of the mass of chromic anhydride is added for dissolving chromic anhydride; alcohol with 10-20% of the theory quantity is slowly added for prereducing chromic anhydride; hydrochloric acid with 1.1-1.3 times the theory quantity and residual alcohol with 90% of the theory quantity are uniformly mixed, and then slowly added to the reaction vessel; stirring and reaction are performed for 1h; a reacted material is evaporated and concentrated until a concentration reaches 45 baume; after the concentration of the material is qualified by evaporation, heating is stopped; natural cooling to a room temperature is performed; crystallization is performed for 8h in a slow stirring state; after the material is crystallized, a chromic chloride hexahydrate product is obtained by centrifugal separation; a mother solution is collected, returns to an evaporation system, and is continued to be condensed; and the product is crystallized and separated again. The method is clean in production, environment-friendly in product and simple in technology; and chromic chloride hexahydrate can replace heavy-pollution hexavalent chromic salt, is widely applied to the industries of electroplating, mordanting, catalysts and the like, and is a revolution of chromic salt development.
Description
Technical field
The invention belongs to the production technical field of chromium chloride hexahydrate, relate in particular to a kind of production method of chromium chloride hexahydrate.
Background technology
Chromium chloride hexahydrate (chemical formula: CrCl
36H
2o) be the deep green crystalline powder, soluble in water, be dissolved in ethanol, be insoluble to ether.Thermal degradation.Be mainly used in the industries such as chromium plating, mordant dyeing, catalyzer.This product is chromic salt, therefore be general chemical, is not subject to control.
Current, Resources for construction saving type, environmentally friendly project, Circular Economy develop in a healthy way, and increase the emphasis that energy saving and environment friendly product has become enterprise development.
The main method for preparing chromium chloride has: the methods such as ethanol reduction chromium chloride processed, carbon ferrochrome chlorination chromium chloride processed, chromoxide green chlorination chromium chloride processed, the molten chromium chloride processed of chromium hydroxide hydrochloric acid acid for chromic trioxide.But because requirements such as technical qualification and product purities, chromic trioxide is the common methods of suitability for industrialized production by ethanol reduction chromium chloride method processed.
Existing method environmental pollution weight, sexavalent chrome is large to the injury of human body.
Summary of the invention
The purpose of the embodiment of the present invention is to provide a kind of production method of chromium chloride hexahydrate, is intended to solve existing method environmental pollution weight, the problem that sexavalent chrome is large to the injury of human body.
The embodiment of the present invention is achieved in that a kind of production method of chromium chloride hexahydrate, and the production method of this chromium chloride hexahydrate comprises the following steps:
Chromic trioxide is added in reaction vessel, add the water dissolution chromic trioxide of chromic anhydride quality 60%-80%, slowly add the alcohol prereduction chromic trioxide of theoretical amount 10%-20%;
The alcohol of the hydrochloric acid of theoretical amount 1.1-1.3 times and residue theoretical amount 90% is mixed to rear slowly adding in reaction vessel, stirring reaction 1 hour;
Completely reacted material by evaporation concentration, is stopped to evaporation after making concentration reach 45 Baumes;
After material concentration evaporation is qualified, stop heating, naturally cool to room temperature crystallization 8 hours under slow whipped state;
After material forms crystallization, obtain the chromium chloride hexahydrate product by centrifugation, mother liquor returns to vapo(u)rization system after collecting, continue concentrated after Crystallization Separation product again.
Further, the production method of this chromium chloride hexahydrate is:
In the enamel reaction still with condenser, the chromic trioxide solution that adds 100Kg60w%, the ethanol 1.5Kg of 95w% was slowly added to retort in 30 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 6Kg ethanol and 190Kg35w% under agitation condition, this process adds in 2 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
Further, the production method of this chromium chloride hexahydrate is:
In the enamel reaction still with condenser, the chromic trioxide solution that adds 200Kg60w%, the ethanol 3Kg of 95w% was slowly added to retort in 40 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 12Kg ethanol and 380Kg35w% under agitation condition, this process adds in 3 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
The production method of chromium chloride hexahydrate provided by the invention, by take chromic trioxide, hydrochloric acid and raw spirit as raw material, be sequentially added into raw material in reaction vessel, after the reaction certain hour, sexavalent chrome is reduced fully, obtain the aqueous solution of chromium chloride, be concentrated to crystallisation by cooling after finite concentration, centrifugation obtains the chromium chloride hexahydrate product.The present invention produces clean, the product environmental protection, and technique is simple, and can replace polluting heavy sexavalence chromic salts and be widely used in electroplating, dying the industries such as matchmaker and catalyzer, be the revolution again of chromic salts development.In addition, chromium chloride hexahydrate of the present invention is chromic salt, can replace the sexavalence chromic salts to be widely used in electroplating, dying the industries such as matchmaker and catalyzer, can effectively alleviate environmental pollution and reduce the injury of sexavalent chrome to human body, be a kind of environmental protection, clean chromic salts product, have wide market outlook and profit to be worth.
The accompanying drawing explanation
Fig. 1 is the schema of the production method of the chromium chloride hexahydrate that provides of the embodiment of the present invention;
Fig. 2 is the schema of the production technique of the chromium chloride hexahydrate that provides of the embodiment of the present invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Fig. 1 shows the production method flow process of chromium chloride hexahydrate provided by the invention.For convenience of explanation, only show part related to the present invention.
The production method of the chromium chloride hexahydrate of the embodiment of the present invention, the production method of this chromium chloride hexahydrate comprises the following steps:
Chromic trioxide is added in reaction vessel, add the water dissolution chromic trioxide of chromic anhydride quality 60%-80%, slowly add the alcohol prereduction chromic trioxide of theoretical amount 10%-20%;
The alcohol of the hydrochloric acid of theoretical amount 1.1-1.3 times and residue theoretical amount 90% is mixed to rear slowly adding in reaction vessel, stirring reaction 1 hour;
Completely reacted material by evaporation concentration, is stopped to evaporation after making concentration reach 45 Baumes;
After material concentration evaporation is qualified, stop heating, naturally cool to room temperature crystallization 8 hours under slow whipped state;
After material forms crystallization, obtain the chromium chloride hexahydrate product by centrifugation, mother liquor returns to vapo(u)rization system after collecting, continue concentrated after Crystallization Separation product again.
As a prioritization scheme of the embodiment of the present invention, the production method of this chromium chloride hexahydrate is:
In the enamel reaction still with condenser, the chromic trioxide solution that adds 100Kg60w%, the ethanol 1.5Kg of 95w% was slowly added to retort in 30 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 6Kg ethanol and 190Kg35w% under agitation condition, this process adds in 2 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
As a prioritization scheme of the embodiment of the present invention, the production method of this chromium chloride hexahydrate is:
In the enamel reaction still with condenser, the chromic trioxide solution that adds 200Kg60w%, the ethanol 3Kg of 95w% was slowly added to retort in 40 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 12Kg ethanol and 380Kg35w% under agitation condition, this process adds in 3 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
As a prioritization scheme of the embodiment of the present invention, chromium chloride hexahydrate makes by the either method of claim 1-3.
Below in conjunction with drawings and the specific embodiments, application principle of the present invention is further described.
As shown in Figure 1, the production method of the chromium chloride hexahydrate of the embodiment of the present invention comprises the following steps:
S101: chromic trioxide is added in reaction vessel, add the water dissolution chromic trioxide of chromic anhydride quality 80%, slowly add the alcohol prereduction chromic trioxide of theoretical amount 20%;
S102: the alcohol of the hydrochloric acid of 1.1 times of theoretical amount and residue theoretical amount 90% is mixed to rear slowly adding in reaction vessel, stirring reaction 1 hour;
S103: completely reacted material by evaporation concentration, is stopped to evaporation after making concentration reach 45 Baumes;
S104: after material concentration evaporation is qualified, stop heating, naturally cool to room temperature crystallization 8 hours under slow whipped state;
S105: after material forms crystallization, by centrifugation, obtain the chromium chloride hexahydrate product, mother liquor returns to vapo(u)rization system after collecting, continue concentrated after Crystallization Separation product again.
The present invention includes the following step:
The first step, reaction process
Chromic trioxide is added in reaction vessel, the water dissolution chromic trioxide that adds chromic anhydride quality 60%-80%, at first the alcohol prereduction chromic trioxide that adds theoretical amount 10%-20%, because of chromic trioxide with react violent and a large amount of heat releases in the alcohol reaction process, therefore need slowly add alcohol, after treating that alcohol adds, by theoretical amount 1.1-1.3, the alcohol of hydrochloric acid doubly and residue theoretical amount 90% mixes and slowly adds in reaction vessel afterwards, because the whole process reaction is violent and a large amount of heatings, therefore reinforced, need slowly evenly to add, and omnidistance the unlatching stirred, after treating that whole materials add, continue to open stirring reaction 1 hour, material is fully reacted, sexavalent chrome is reduced fully,
Second step, evaporization process, by evaporation concentration, stop evaporation after making concentration reach 45 Baumes by completely reacted material;
The 3rd step, Crystallization Procedure, after material concentration evaporation is qualified, stop heating, naturally cools to room temperature crystallization 8 hours under slow whipped state;
The 4th step, the finished product operation: after material forms crystallization, by centrifugation, obtain the chromium chloride hexahydrate product, mother liquor returns to vapo(u)rization system after collecting, continue concentrated after Crystallization Separation product again.
The specific embodiment of the present invention: as shown in Figure 2
Embodiment 1
In the enamel reaction still with condenser, the chromic trioxide solution that adds 100Kg60w%, the ethanol 1.5Kg of 95w% was slowly added to retort in 30 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 6Kg ethanol and 190Kg35w% under agitation condition, this process approximately adds in 2 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation;
The product result of determination is salable product
Embodiment 2
In the enamel reaction still with condenser, the chromic trioxide solution that adds 200Kg60w%, the ethanol 3Kg of 95w% was slowly added to retort in 40 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 12Kg ethanol and 380Kg35w% under agitation condition, this process approximately adds in 3 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
The product result of determination is acceptable end product
Chromium chloride of the present invention is that chromic salt can replace the sexavalence chromic salts to be widely used in electroplating, dying the industries such as matchmaker and catalyzer, can effectively alleviate environmental pollution and reduce the injury of sexavalent chrome to human body.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. the production method of a chromium chloride hexahydrate, is characterized in that, the production method of this chromium chloride hexahydrate comprises the following steps:
Chromic trioxide is added in reaction vessel, add the water dissolution chromic trioxide of chromic anhydride quality 60%-80%, slowly add the alcohol prereduction chromic trioxide of theoretical amount 10%-20%;
The alcohol of the hydrochloric acid of theoretical amount 1.1-1.3 times and residue theoretical amount 90% is mixed to rear slowly adding in reaction vessel, stirring reaction 1 hour;
Completely reacted material by evaporation concentration, is stopped to evaporation after making concentration reach 45 Baumes;
After material concentration evaporation is qualified, stop heating, naturally cool to room temperature crystallization 8 hours under slow whipped state;
After material forms crystallization, obtain the chromium chloride hexahydrate product by centrifugation, mother liquor returns to vapo(u)rization system after collecting, continue concentrated after Crystallization Separation product again.
2. the production method of chromium chloride hexahydrate as claimed in claim 1, is characterized in that, the production method of this chromium chloride hexahydrate is:
In the enamel reaction still with condenser, the chromic trioxide solution that adds 100Kg60w%, the ethanol 1.5Kg of 95w% was slowly added to retort in 30 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 6Kg ethanol and 190Kg35w% under agitation condition, this process adds in 2 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
3. the production method of chromium chloride hexahydrate as claimed in claim 1, is characterized in that, the production method of this chromium chloride hexahydrate is:
In the enamel reaction still with condenser, the chromic trioxide solution that adds 200Kg60w%, the ethanol 3Kg of 95w% was slowly added to retort in 40 minutes, again by slowly adding reactor after the mixed in hydrochloric acid of 12Kg ethanol and 380Kg35w% under agitation condition, this process adds in 3 hours, continue reaction and within 1 hour, make sexavalent chrome be reduced fully, cooling spontaneous nucleation after evaporation concentration, then obtain the chromium chloride hexahydrate product through centrifugation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104192906A (en) * | 2014-08-29 | 2014-12-10 | 四川省银河化学股份有限公司 | Method for preparing chromium trichloride hexahydrate by utilizing sodium chromate |
| CN105883920A (en) * | 2014-10-16 | 2016-08-24 | 山西国润制药有限公司 | Preparation method of chromium trichloride |
| CN107529519A (en) * | 2017-10-12 | 2018-01-02 | 北京科技大学 | A kind of yolk shell structure CrF3·3H2O preparation method |
| CN110817960A (en) * | 2019-12-26 | 2020-02-21 | 四川省银河化学股份有限公司 | Method for preparing chromium chloride hexahydrate by using sodium chromate |
-
2013
- 2013-08-23 CN CN2013103746974A patent/CN103466707A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 丁翼: "《铬化合物生产与应用》", 28 February 2003, 化学工业出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104192906A (en) * | 2014-08-29 | 2014-12-10 | 四川省银河化学股份有限公司 | Method for preparing chromium trichloride hexahydrate by utilizing sodium chromate |
| CN104192906B (en) * | 2014-08-29 | 2016-02-10 | 四川省银河化学股份有限公司 | A kind of Sodium chromate prepares the method for chromium chloride hexahydrate |
| CN105883920A (en) * | 2014-10-16 | 2016-08-24 | 山西国润制药有限公司 | Preparation method of chromium trichloride |
| CN107529519A (en) * | 2017-10-12 | 2018-01-02 | 北京科技大学 | A kind of yolk shell structure CrF3·3H2O preparation method |
| CN107529519B (en) * | 2017-10-12 | 2019-04-09 | 北京科技大学 | A kind of yolk-shell structure CrF3·3H2The preparation method of O |
| CN110817960A (en) * | 2019-12-26 | 2020-02-21 | 四川省银河化学股份有限公司 | Method for preparing chromium chloride hexahydrate by using sodium chromate |
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Application publication date: 20131225 |