CN103466708B - Method for producing basic chrome sulphate with dichromiumtris (chromate) slag - Google Patents
Method for producing basic chrome sulphate with dichromiumtris (chromate) slag Download PDFInfo
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- CN103466708B CN103466708B CN201310374941.7A CN201310374941A CN103466708B CN 103466708 B CN103466708 B CN 103466708B CN 201310374941 A CN201310374941 A CN 201310374941A CN 103466708 B CN103466708 B CN 103466708B
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- sodium dichromate
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- slag
- urea
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Abstract
The invention discloses a method for producing basic chrome sulphate with dichromiumtris (chromate) slag. The method for producing basic chrome sulphate with the dichromiumtris (chromate) slag comprises the following steps of completely dissolving the dichromiumtris (chromate) slag with concentrated sulfuric acid, that is, adding 1.93t sulfuric acid per ton of Cr2O3 according to a Cr2O3 content in a raw material, adding 0.37-0.42t urea per ton of Cr2O3 to prepare a 10% urea solution and a 50% sodium bichromate solution, slowly adding the prepared urea solution and the sodium bichromate solution into acid soluble dichromiumtris (chromate) slag slurry, heating the slurry to be boiled, performing continuous reaction for 2-3h, filtering the reacted slurry, and after alkalinity of liquid basic chrome sulphate is detected to be qualified, obtaining a basic chrome sulphate finish product through a spray dryer. The method takes the waste dichromiumtris (chromate) slag as a raw material, is environment-friendly, saves resources, reduces unit consumption, produces obvious economic benefits, and provides an energy-saving, environment-friendly and synergetic novel production technology.
Description
Technical field
The invention belongs to chromium sulphate production technical field, particularly relate to a kind of method utilizing chromic acid chromium slag to produce basic chromium sulfate.
Background technology
Basic chromium sulfate is mainly used in leather retanning agent, and the quality of leather is generally just the quality of leather tanning agent and the technique of leather tanning agent processing, and basic chromium sulfate and sodium dichromate, chromic anhydride, chromoxide green are listed as the large range of product of chromic salts four;
The molecular formula of basic chromium sulfate represents with following general formula: Cr (OH) n (SO4) 0.5 (3-n), as n=3, represents chromium hydroxide (Cr(OH) 3), be chromium sulphate (Cr during n=0
2(SO
4)
3), custom basicity represents basic chromium sulfate basicity, also be the per-cent that in basic chromium sulfate, hydroxide radical (OH-) equivalents accounts for anion equivalents sum 3 in molecule, that is: basicity=n/3*100%, the basicity of commodity basic chromium sulfate is generally at 33-42%, be equivalent to equivalents n=1-1.3 hydroxy in molecule, when during n=1, basicity is 33%, n=1.3 and basicity be 42%;
Traditional basic chromium sulfate production method directly with sodium dichromate and sucrose for raw material is produced, unit consumption is high, and environmental benefit is low, is unfavorable for energy-saving and emission-reduction.
Summary of the invention
The object of the embodiment of the present invention is to provide a kind of method utilizing chromic acid chromium slag to produce basic chromium sulfate, and the unit consumption being intended to solve traditional basic chromium sulfate production method existence is high, and environmental benefit is low, is unfavorable for the problem of energy-saving and emission-reduction.
The embodiment of the present invention is achieved in that a kind of method utilizing chromic acid chromium slag to produce basic chromium sulfate, and this method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
Step one, by completely acid-soluble for the chromic acid chromium slag vitriol oil, namely according to Cr in raw material
2o
3content, the sulfuric acid quality that Cr2O3 per ton need add is 1.93 tons;
Step 2, Cr per ton
2o
3the urea quality that need add is 0.37 ~ 0.42 ton, the configuration urea soln of 10% and the sodium dichromate solution of 50%;
Step 3, slowly adds the urea soln configured and sodium dichromate solution in acid-soluble chromic acid chromium slag charge liquid;
Step 4, heating feed liquid is to boiling, and successive reaction 2 ~ 3 hours;
Step 5, filters completely reacted feed liquid, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
Further, in step 2,1.3 ~ 1.5 times of configuration urea solns of the theoretical amount of the basic chromium sulfate that urea quality generates according to reaction, namely sodium dichromate can be sodium dichromate finished product, also can use the sodium dichromate 99 feed liquid of sodium dichromate production process middle and high concentration.
Further, in step 3, the ratio of the add-on of chromic acid chromium slag and the add-on of sodium dichromate 1:1 in mass ratio adds.
Further, this method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
The first step, by 500Kg chromic acid chromium slag, Cr
2o
3content: 8.58%, with 610Kg industry vitriol oil content 93.5%, completely acid-soluble;
Second step, is dissolved into 110Kg urea in 1100Kg water and is configured to urea soln, is dissolved in 1000Kg water by 500Kg sodium dichromate and is configured to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 2 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
Further, this method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
The first step, by 500Kg chromic acid chromium slag, Cr
2o
3content: 8.58%, with 615Kg industry vitriol oil content 93.5%, completely acid-soluble;
Second step, is dissolved into 119Kg urea in 1190Kg water and is configured to urea soln, is dissolved in 1000Kg water by 500Kg sodium dichromate and is configured to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 2.5 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
Further, this method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
The first step, by 500Kg chromic acid chromium slag, Cr
2o
3content: 8.58%, completely acid-soluble with 620Kg industry vitriol oil content 93.5%;
Second step, is dissolved into 125Kg urea in 1250Kg water and is configured to urea soln, and a sodium dichromate 99 content of picking up the car is the sodium dichromate acidizing fluid 400L of 1250g/l, then adds 800Kg water and be diluted to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 3 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
Further, this method utilizing chromic acid chromium slag to produce basic chromium sulfate is obtained by the arbitrary described preparation method of claim 1-6.
The method utilizing chromic acid chromium slag to produce basic chromium sulfate provided by the invention, by replacing part sodium dichromate with the useless chromic acid chromium slag of part for raw material on the basis of former technique, replacing sucrose with urea, namely reducing unit consumption with this, produce environmental benefit again, serve positive energy-saving and emission-reduction exemplary role.In addition, the present invention for raw material, both solved environmental issue, again saving resource with discarded chromic acid chromium slag, reduced unit consumption, produced obvious economic benefit, provide the novel production process of a kind of energy-saving and environmental protection, synergy.
Accompanying drawing explanation
Fig. 1 is that the chromic acid chromium slag that utilizes that the embodiment of the present invention provides produces the schema of the method for basic chromium sulfate.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be not intended to limit the present invention.
Fig. 1 shows the flow process utilizing chromic acid chromium slag to produce the method for basic chromium sulfate provided by the invention.For convenience of explanation, illustrate only part related to the present invention.
The chromic acid chromium slag that utilizes of the embodiment of the present invention produces the method for basic chromium sulfate, and this method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
Step one, by completely acid-soluble for the chromic acid chromium slag vitriol oil, namely according to Cr in raw material
2o
3content, the sulfuric acid quality that Cr2O3 per ton need add is 1.93 tons;
Step 2, Cr per ton
2o
3the urea quality that need add is 0.37 ~ 0.42 ton, the configuration urea soln of 10% and the sodium dichromate solution of 50%;
Step 3, slowly adds the urea soln configured and sodium dichromate solution in acid-soluble chromic acid chromium slag charge liquid;
Step 4, heating feed liquid is to boiling, and successive reaction 2 ~ 3 hours;
Step 5, filters completely reacted feed liquid, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
As a prioritization scheme of the embodiment of the present invention, in step 2,1.3 ~ 1.5 times of configuration urea solns of the theoretical amount of the basic chromium sulfate that urea quality generates according to reaction, namely sodium dichromate can be sodium dichromate finished product, also can use the sodium dichromate 99 feed liquid of sodium dichromate production process middle and high concentration.
As a prioritization scheme of the embodiment of the present invention, in step 3, the ratio of the add-on of chromic acid chromium slag and the add-on of sodium dichromate 1:1 in mass ratio adds.
Below in conjunction with drawings and the specific embodiments, application principle of the present invention is further described.
As shown in Figure 1, the method utilizing chromic acid chromium slag to produce basic chromium sulfate of the embodiment of the present invention comprises the following steps:
S101: by completely acid-soluble for the chromic acid chromium slag vitriol oil, namely according to Cr in raw material
2o
3content, the sulfuric acid quality that Cr2O3 per ton need add is 1.93 tons;
S102: Cr per ton
2o
3the urea quality that need add is 0.37 ~ 0.42 ton, the configuration urea soln of 10% and the sodium dichromate solution of 50%;
S103: the urea soln configured and sodium dichromate solution are slowly added in acid-soluble chromic acid chromium slag charge liquid;
S104: heating feed liquid is to boiling, and successive reaction 2 ~ 3 hours;
S105: filter completely reacted feed liquid, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
Concrete steps of the present invention are:
Step one, by completely acid-soluble for the chromic acid chromium slag vitriol oil; The vitriol oil quality added adds sulfuric acid, namely according to Cr in raw material according to the theoretical amount of the basic chromium sulfate that reaction generates
2o
3content, Cr per ton
2o
3the sulfuric acid quality that need add is 1.93 tons.
Step 2,1.3 ~ 1.5 times of configuration urea solns of the theoretical amount of the basic chromium sulfate that urea quality generates according to reaction, namely according to Cr in raw material
2o
3content, Cr per ton
2o
3the urea quality that need add is 0.37 ~ 0.42 ton.The configuration urea soln of 10% and the sodium dichromate solution of 50%; Namely sodium dichromate can be sodium dichromate finished product, also can use the sodium dichromate 99 feed liquid of sodium dichromate production process middle and high concentration;
Step 3, slowly adds the urea soln configured and sodium dichromate solution in acid-soluble chromic acid chromium slag charge liquid; The ratio of the add-on of chromic acid chromium slag and the add-on of sodium dichromate 1:1 in mass ratio adds;
Step 4, heating feed liquid is to boiling, and successive reaction 2 ~ 3 hours;
Step 5, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.Industry basic chromium sulfate standard is as shown in table 1:
The industrial basic chromium sulfate standard of table 1:
The specific embodiment of the present invention:
Embodiment 1
The first step, by 500Kg chromic acid chromium slag (Cr
2o
3content: 8.58%) completely acid-soluble with the 610Kg industry vitriol oil (content 93.5%);
Second step, is dissolved into 110Kg urea in 1100Kg water and is configured to urea soln, is dissolved in 1000Kg water by 500Kg sodium dichromate and is configured to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 2 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.Finished product total analysis result is as follows:
| Content | Basicity | Iron | Water-insoluble | Sexavalent chrome |
| 21.85% | 40.19% | 0.089% | 0.091% | 0.00030% |
Through inspection, product meets basic chromium sulfate II series products standard.
Embodiment 2
The first step, by 500Kg chromic acid chromium slag (Cr
2o
3content: 8.58%) completely acid-soluble with the 615Kg industry vitriol oil (content 93.5%);
Second step, is dissolved into 119Kg urea in 1190Kg water and is configured to urea soln, is dissolved in 1000Kg water by 500Kg sodium dichromate and is configured to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 2.5 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.Finished product total analysis result is as follows:
| Content | Basicity | Iron | Water-insoluble | Sexavalent chrome |
| 22.08% | 37.25% | 0.092% | 0.096% | 0.00026% |
Through inspection, product meets basic chromium sulfate II series products standard.
Embodiment 3
The first step, by 500Kg chromic acid chromium slag (Cr
2o
3content: 8.58%) completely acid-soluble with the 620Kg industry vitriol oil (content 93.5%);
Second step, is dissolved into 125Kg urea in 1250Kg water and is configured to urea soln, and a sodium dichromate 99 content of picking up the car is the sodium dichromate acidizing fluid 400L of 1250g/l, then adds 800Kg water and be diluted to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 3 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
Finished product total analysis result is as follows:
| Content | Basicity | Iron | Water-insoluble | Sexavalent chrome |
| 23.06% | 35.62% | 0.090% | 0.085% | 0.00020% |
Through inspection, product meets basic chromium sulfate II series products standard.
Principle of work of the present invention is:
The present invention replaces part sodium dichromate with the useless chromic acid chromium slag of part for raw material on the basis of former technique, replaces sucrose, namely reduce unit consumption, produce environmental benefit again, serve positive " energy-saving and emission-reduction " exemplary role with this with urea.Chromic acid chromium slag in the present invention is originated and is that raw material production basic chromium sulfate reaction principle is as follows with chromic acid chromium slag:
1, the generation of chromic acid chromium:
The reaction of sodium pyrosulfate suspension liquid and vanadium removal liquid has acidifying, precipitation and precipitation to transform three parts:
2Na2CrO4+NaHSO4==Na2Cr2O7+2Na2SO4+H2O ①
Water-soluble chromium sulphate (Cr2(SO4) 3 in sodium pyrosulfate) or bisulphate chromium (Cr(HSO4) 3) react generate chromic acid chromium (Cr2O3 ﹒ CrO3 ﹒ xH2O) with Sodium chromate.
2Cr2（SO4）3+Na2CrO4+（x+5）H2O==2Cr2O3﹒CrO3﹒xH2O+2NaHSO4+4H2SO4 ②
4Cr（HSO4）3+Na2CrO4+（x+5）H2O==2Cr2O3﹒CrO3﹒xH2O+2NaHSO4+10H2SO4 ③
Water-insoluble chromium sodium sulphate (Na3Cr(SO4) 3 in sodium pyrosulfate) change the chromic acid chromium of more indissoluble into:
4Na3Cr（SO4）3+Na2CrO4+（x+5）H2O==2Cr2O3﹒CrO3﹒xH2O+10NaHSO4+2H2SO4 ④
Because of chromium sodium sulphate indissoluble, therefore above formula conversion rate is slower.
2, the production of basic chromium sulfate:
Replace sodium dichromate 99 mother liquor with chromic acid chromium slag, with sulfuric acid acidation, add saltcake and regulate chromium content and basicity, then add Urea reduction, last spraying dry and the powdery basic chromium sulfate made.Main chemical reactions equation is:
2Cr2O3﹒CrO3﹒xH2O+H2SO4==Cr2（SO4）3+H2Cr2O7+xH2O⑤
8Na2Cr2O7﹒2H2O+24H2SO4+C12H22O11==16Cr（OH）SO4+12CO2+29H2O+8Na2SO4 ⑥
The present invention for raw material, both solved environmental issue, again saving resource with discarded chromic acid chromium slag, reduced unit consumption, produced obvious economic benefit, provide the novel production process of a kind of energy-saving and environmental protection, synergy.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. utilize chromic acid chromium slag to produce a method for basic chromium sulfate, it is characterized in that, this method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
Step one, by completely acid-soluble for the chromic acid chromium slag vitriol oil, namely according to Cr2O3 content in raw material, the sulfuric acid quality that Cr2O3 per ton need add is 1.93 tons;
Step 2, the urea quality that Cr2O3 per ton need add is 0.37 ~ 0.42 ton, the configuration urea soln of 10% and the sodium dichromate solution of 50%;
Step 3, slowly adds the urea soln configured and sodium dichromate solution in acid-soluble chromic acid chromium slag charge liquid;
Step 4, heating feed liquid is to boiling, and successive reaction 2 ~ 3 hours;
Step 5, filters completely reacted feed liquid, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer;
In step 2,1.3 ~ 1.5 times of configuration urea solns of the theoretical amount of the basic chromium sulfate that urea quality generates according to reaction, namely sodium dichromate can be sodium dichromate finished product, also can use the sodium dichromate 99 feed liquid of sodium dichromate production process middle and high concentration;
In step 3, the ratio of the add-on of chromic acid chromium slag and the add-on of sodium dichromate 1:1 in mass ratio adds;
This method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
The first step, by 500Kg chromic acid chromium slag, Cr2O3 content: 8.58%, with 610Kg industry vitriol oil content 93.5%, completely acid-soluble;
Second step, is dissolved into 110Kg urea in 1100Kg water and is configured to urea soln, is dissolved in 1000Kg water by 500Kg sodium dichromate and is configured to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 2 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer;
This method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
The first step, by 500Kg chromic acid chromium slag, Cr2O3 content: 8.58%, with 615Kg industry vitriol oil content 93.5%, completely acid-soluble;
Second step, is dissolved into 119Kg urea in 1190Kg water and is configured to urea soln, is dissolved in 1000Kg water by 500Kg sodium dichromate and is configured to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 2.5 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer;
This method utilizing chromic acid chromium slag to produce basic chromium sulfate comprises the following steps:
The first step, by 500Kg chromic acid chromium slag, Cr2O3 content: 8.58%, completely acid-soluble with 620Kg industry vitriol oil content 93.5%;
Second step, is dissolved into 125Kg urea in 1250Kg water and is configured to urea soln, and a sodium dichromate 99 content of picking up the car is the sodium dichromate acidizing fluid 400L of 1250g/l, then adds 800Kg water and be diluted to sodium dichromate solution;
3rd step, slowly joins in acid-soluble good chromic acid chromium slag charge liquid by the urea soln configured and sodium dichromate solution;
4th step, heating feed liquid is to boiling, and successive reaction 3 hours;
5th step, filters completely reacted feed liquid, and filtrate is liquid basic chromium sulfate, detect liquid basic chromium sulfate basicity qualified after, namely obtain basic chromium sulfate finished product by spray-dryer.
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|---|---|---|---|
| CN201310374941.7A CN103466708B (en) | 2013-08-23 | 2013-08-23 | Method for producing basic chrome sulphate with dichromiumtris (chromate) slag |
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|---|---|---|---|
| CN201310374941.7A CN103466708B (en) | 2013-08-23 | 2013-08-23 | Method for producing basic chrome sulphate with dichromiumtris (chromate) slag |
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| CN103936073B (en) * | 2014-04-30 | 2015-09-30 | 东北大学 | A kind of magnochromite sulphuric leachate produces the method for basic chromium sulfate |
| CN104609473B (en) * | 2014-12-18 | 2016-08-24 | 北京矿冶研究总院 | Method for preparing basic chromium sulfate from chromium phosphate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4332584A (en) * | 1979-04-20 | 1982-06-01 | Systems Consultants, Inc. | Recovery of potential energy and chromium values from leather tannery wastes |
| CN1099727A (en) * | 1993-09-01 | 1995-03-08 | 中国科技开发院化工开发所 | Making method for basic chromium sulfate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5365291A (en) * | 1976-11-25 | 1978-06-10 | Showa Denko Kk | Production of basic chromium sulfate |
-
2013
- 2013-08-23 CN CN201310374941.7A patent/CN103466708B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4332584A (en) * | 1979-04-20 | 1982-06-01 | Systems Consultants, Inc. | Recovery of potential energy and chromium values from leather tannery wastes |
| CN1099727A (en) * | 1993-09-01 | 1995-03-08 | 中国科技开发院化工开发所 | Making method for basic chromium sulfate |
Non-Patent Citations (2)
| Title |
|---|
| "铬酸铬渣生产铬鞣剂过程中除铁研究";陈雪梅;《中国皮革》;20091031;第38卷(第19期);第1页左栏倒数8-6行、第2页1.2节 * |
| 丁冀."蔗糖还原法制备碱式硫酸铬".《铬化合物生产与应用》.化学工业出版社,2003,231-232. * |
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