CN105016388B - The environmentally protective manufacture chromium compound technique of carbon ferrochrome clean energy-saving - Google Patents
The environmentally protective manufacture chromium compound technique of carbon ferrochrome clean energy-saving Download PDFInfo
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- CN105016388B CN105016388B CN201410168931.2A CN201410168931A CN105016388B CN 105016388 B CN105016388 B CN 105016388B CN 201410168931 A CN201410168931 A CN 201410168931A CN 105016388 B CN105016388 B CN 105016388B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention relates to a kind of environmentally protective manufacture chromium compound techniques of carbon ferrochrome clean energy-saving, the invented technology is advanced, energy conservation and environmental protection, high temperature and pressure is not necessarily to without fire coal, the products such as chromium compound, pigment, new energy, silicon-carbon battery new material are disposably produced by raw material liquid phase method of ferrochrome, a series of new high-end industrial chains are formed, the situation that original product purpose is single, production is simple is revolutionized；The production technology that original chromate compound production generates the high pollution backwardness big to environmental hazard is changed, the production of chromium compound is made to go on energy conservation and environmental protection, the development of high benefit；The development of ferrochrome Diversification and application field are greatly expanded, Enterprise International Competition is greatly strengthened, promotes national industry optimization and upgrading and development, is of great significance.
Description
Technical field
The present invention relates to a kind of environmentally protective manufacture chromium compound techniques of carbon ferrochrome clean energy-saving, and belonging to metallurgic product is
Raw material manufactures the technical field of chromium compound, iron pigment, new material, new energy.
Background technique
As international economic integration paces are accelerated, competition among enterprises are growing more intense, and enterprise will be in fierce international competition
Acquire the survival and development, it is necessary to the adjusting and optimizing industrial structure, Economic Development Mode Conversion accelerate to eliminate the backward production facilities, guidance and
It pushes resource to assemble to strong industry and new and high technology, pushes Industry Structure optimization and upgrading.Enterprise should add from global view
Big Innovation Input, enhances the capacity for independent innovation, and introduces high-new efficient science and technology, improves overall technology level, comprehensive diversification hair
Exhibition, enhances one's market competitiveness.Development & production high-tech new material, new energy, the product of environmental protection and energy saving meet international and domestic to new
The demand of product new material.
Sexavalence chromic salts is reduced to chromic salt using reducing agent by original chromic salt production method.Domestic and international scale
Change sexavalence chrome salt production enterprise 22, wherein 12, China, is all to use to have calcium roasting and calcium-free roasting as raw material using chromite
Method produces chromate through high-temperature roasting, contains harmful hexavalent chromium in the fume gases that roasting method production generates, and generates a large amount of
Toxic chromium slag, waste water generate very big harm to environment and the mankind.Government of chromium salt production state of the world, scientific research institution, universities and colleges, enterprise
The departments such as industry group, individual all put into a large amount of manpower, financial resources, material resources and are dedicated to innovation, are intended to seek a kind of new process new
Method substitutes original chromic salts roasting method.
Several years ago in great demand to chromic salts due to international market, high price is run all the way in chromic salts market, domestic chromic salts production capacity
22.6 ten thousand tons from 2008 rapidly increase to current 360,000 tons, account for the 40% of international market, and domestic consumption amount also reaches complete
The 39% of ball, China become chromium salt production, consumption and big export country.However, since 2012, it is whole weak by international market
Influence, the outlets such as China's chromic salts product and electroplated product, ceramics, dyeing and printing products are seriously obstructed, export volume downlink.It is same with this
When, it is influenced by National Macroscopic economic adjustment policy and environmentally friendly severe situation, chromic salts down-stream enterprise stops production one after another, limits the production, domestic
There is severe atrophy in the chromic salts market demand.
Currently, China's chrome salt production enterprise cost is projecting, suffer great loss, technique falls behind, and shuffles wait raise speed.Expert points out,
According to demand both domestic and external and international trend, it is necessary to technological progress is relied on, using the new technology of advanced clean energy-saving environmental protection
New process new method, Economic Development Mode Conversion push Chrome Salt Industry industry restructuring and optimization and upgrading, keep Chrome Salt Industry early
Go on sound development road high in technological content, good in economic efficiency, low in resources consumption, low in the pollution of the environment, that safety is secure day.
Chromic salts enterprise is entirely to generate a large amount of chromium using having calcium or few calcium method of roasting production chromate both at home and abroad now
Slag, processing cost is high, and processing is difficult, the serious development and industrial upgrading for restricting enterprise.Some new processes that China encourages but can not
Promote and apply: the potassium system sub-molten salt liquid phase oxidation that the process study of 1. Chinese Academy of Sciences is invented is because needing reaction temperature height, potash
Dosage is big, reaction vessel manufacture is difficult, it is at high cost can not industrial applications；2. by Chongqing Minfeng Chemical Co., Ltd.'s invention
" technique that three compartment catalysis oxidations prepare dissolubility chromate ", application number: 201110261747.9, publication number:
CN102320661A, publication date: 2012.01.18, the prosperous first chemical industry in maximum potassium permanganate manufacturing enterprise Chongqing is invented in the world
" a kind of preparation process of Continuous Liquid Phase oxidation reaction tower production chromate ", application number: 201110035642.1, publication number:
CN102139921A, publication date: 2011.08.03, these methods all need high temperature and pressure, a large amount of alkali are needed in production, to container
It is required that high, reaction vessel cost is high, damages greatly in production process to container, while being easy to produce security risk.Due to production
It is at high cost, only single product sodium chromate, while it is difficult to generate toxic chromic wastes disposal, it is difficult to industrialized production.
Therefore, it is badly in need of a kind of environmentally protective, clean energy-saving, advanced practical chromium compounds processing condition and method.
Summary of the invention
It is an object of the invention to economize on resources and the energy, cost is reduced, the chromium of high-quality is produced using ferrochrome as raw material
Compound and iron pigment, intensive diversification innovation and development form high-end product industrial chain, promote scientific and technological economy and society hair
Exhibition.
The purpose of the present invention is reached by following measure:
1. a kind of environmentally protective manufacture chromium compound technique of carbon ferrochrome clean energy-saving, it is characterised in that: wear into ferrochrome
Fine powder is put into reaction kettle, and acid adding dissolves ferrochrome, and extraordinary substance heating reaction is added, product is made, chromium compounds: chromium sulfate, chlorine
Change chromium, chromium oxide, chromium hydroxide, chromate, iron pigment: ferrous oxalate, iron hydroxide, barba hispanica, fervam, silicon, carbon, hydrogen
Gas；
2. raw material ferrochrome is that high carbon ferro-chrome, medium carbon ferrochrome or low-carbon ferrochromium wear into 50 mesh or more carefully according to claim 1
Powder (or carbon ferrochrome is taken to smelt the melting above fine powder of 50 mesh) or chromite or trivalent chromium compound and mixture, are put into reaction
In kettle, enough hydrochloric acid or sulfuric acid is added, 15 DEG C -120 DEG C of heating is sufficiently stirred, and reaction dissolution makes ferrochrome generate ion completely
(Cr3+、Fe2+) solution, hydrogen is collected, product new energy hydrogen is made；
3. making soluble substance become ion according to water is added in claim 2 solution, contain Cr3+、Fe2+Sediment in solution
For Si, suspended matter C, solution is filtered respectively, obtains filtrate and filter residue, filter residue is washed, separates, dry, be made product Si and
C, product Si produce polysilicon and monocrystalline silicon again, and filtrate is containing Cr3+、Fe2+Solution；
4. according to extraordinary substance is added in claim 3 filtrate: alkali and Sodium Dimethyldithiocarbamate, potassium ferrocyanide, potassium ferricyanide, a kind of in oxalic acid
Or it is two or more, make Fe2+It is precipitated as FeC completely2O, fervam, barba hispanica are filtered, washed, dry, and product F eC is made2O4, Fu Mei
Iron, barba hispanica, filtrate Cr3+Solution；
5. according to Cr in claim 43+Solution produces different product；
(1).Cr3+Solution produces chrome tanning agent or trivalent chromium plating solution；
(2).Cr3+Solution evaporation, crystallization, separation, dry obtained product chromic salt；
(3).Cr3+Carbonate, bicarbonate, hydroxide, ammonium hydroxide are added in solution, makes Cr3+It is precipitated as Cr completely
(OH)3, it is filtered, washed, crystallizes, dries, product chromium hydroxide is made, the oxidation of product three two is made in chromium hydroxide high-temperature calcination
Chromium；
(4).Cr3+Extraordinary reactive material: percarbonate (X is added in solution2CO4), persulfate (X2S2O8), hydrogen peroxide
(H2O2), oxygen (O2), peroxide salt (X2O2), permanganate (XMnO4), hypochlorite (XCIO), carbonate (X2CO3), alkali
(XOH), agitating and heating oxidation reaction makes Cr in solution3+It is oxidized to Cr6+, chromatedsolution (CrO is made4 2-) or bichromate
Solution C r2O7 2-；
A. by chromatedsolution (CrO4 2-) or dichromate solution (Cr2O7 2-), evaporative crystallization separates, and it is dry, it is made and produces
Product chromate or bichromate；
B. chromatedsolution (CrO4 2-) in be added acid acidification (sulfuric acid process, carbonizatin method, electrolysis method) make chromatedsolution
(CrO4 2-) dichromate solution (Cr is generated completely2O7 2-), product bichromate is made in evaporative crystallization, separation, drying；
6, according to claim 3 filtrate Fe2+、Cr3+In solution or in claim 4 solution, extraordinary reflection substance is added:
Percarbonate (X2CO4), persulfate (X2S2O8), hydrogen peroxide (H2O2), oxygen (O2), peroxide salt (X2O2), permanganate
(XMnO4), hypochlorite (XCIO), carbonate (X2CO3), alkali (XOH), agitating and heating oxidation reaction makes Cr in solution3+Oxidation
For Cr6+, chromatedsolution (CrO is made4 2-) or dichromate solution Cr2O7 2-, make Fe in solution2+It is precipitated as Fe (OH) completely3；
(1) is by chromatedsolution (CrO4 2-) or dichromate solution (Cr2O7 2-), evaporative crystallization separates, and it is dry, it is made
Product chromate or bichromate；
(2) chromatedsolution (CrO4 2-) in be added acid acidification (sulfuric acid process, carbonizatin method, electrolysis method) make chromatedsolution
(CrO4 2-) dichromate solution (Cr is generated completely2O7 2-), product bichromate is made in evaporative crystallization, separation, drying；
(3) Fe containing Cr VI (OH)3Middle addition acid, adds reducing agent FeSO4、Na2SO3、NaHSO3、Na2S2O5、
Na2S makes Cr6+It is reduced to Cr3+, alkali is added and generates Fe (OH)3With Cr (OH)3Precipitating, separates, is filtered, washed, drying obtained product
Fe(OH)3With Cr (OH)3。
In order to preferably make this inventive technique implement industrialized production as soon as possible, tried on June 28th, 2013
Test production.
Specific embodiment
1. high carbon ferro-chrome 1000kg is worn into the above fine powder of 200 mesh, it is put into reaction kettle, enough sulfuric acid is added
3000kg, 15 DEG C -100 DEG C of heating are sufficiently stirred, and reaction dissolution makes ferrochrome generate ion (Cr completely3+、Fe2+) solution, it collects
Product new energy 40kg hydrogen is made in hydrogen；
So that soluble substance is become ion 2. water is added in solution, contains Cr3+、Fe2+Sediment is Si in solution, and suspended matter is
Solution is filtered respectively, obtains filtrate and filter residue by C, and filter residue is washed, is separated, dry, and product Si:30kg and C:70kg is made, and is produced
Product Si produces polysilicon and monocrystalline silicon again, and filtrate is containing Cr3+、Fe2+Solution and micro metal ion；
3. oxalic acid 650Kg is added in filtrate makes Fe2+It is precipitated as FeC completely2O4, it is filtered, washed, crystallizes, dries, is made and produces
Product FeC2O4: 1100kg, filtrate Cr3+Solution and microelement add Sodium Dimethyldithiocarbamate 0.05kg, remove other micro metals
Ion filters containing Cr3+Filtrate；
4. according to Cr in step 33+Solution produces different product；
(1).Cr3+Product chromium sulfate 1500kg is made in solution evaporation drying；
(2).Cr3+Sodium hydroxide 500kg is added in solution, makes Cr3+It is precipitated as Cr (OH)3, it is filtered, washed, crystallize, does
Dry, product chromium hydroxide is made: product chrome green: 310kg is made in 420kg, chromium hydroxide high-temperature calcination；
(3).Cr3+Extraordinary reflection substance is added in solution: sodium peroxydisulfate, peroxide salt sodium, sodium carbonate 300kg, stirring add
Thermal oxidative reaction makes Cr in solution3+It is oxidized to Cr6+, chromium acid sodium solution is made, by chromium acid sodium solution, evaporative crystallization is separated, and is done
It is dry, product sodium chromate 350kg. is made
5. producing new energy hydrogen 40kg according to process above, new energy battery material: ferrous oxalate 1100kg, silicon
30kg, carbon 70kg, chromium sulfate 1500kg, chromium oxide 310kg, chromium hydroxide 420kg.
It facts have proved that the invented technology is advanced, energy conservation and environmental protection is not necessarily to high temperature and pressure without coal-fired, using ferrochrome as raw material liquid phase
Method disposably produces the products such as chromium compound, pigment, new energy, new energy silicon-carbon battery material, forms a series of new height
Industrial chain is held, the situation that original product purpose is single, production is simple is revolutionized；It is raw to change original chromate compound
The production technology for generating the high pollution backwardness big to environmental hazard, makes the production of chromium compound go on energy conservation and environmental protection, high benefit
Development；The development of ferrochrome Diversification and application field are greatly expanded, Enterprise International Competition is greatly strengthened,
Promote national industry optimization and upgrading and development, is of great significance.
Claims (1)
1. a kind of environmentally protective manufacture chromium compound technique of carbon ferrochrome clean energy-saving, it is characterised in that: ferrochrome is worn into fine powder,
Be put into reaction kettle, acid adding dissolves ferrochrome, extraordinary substance heating reaction is added, product is made, chromium compounds: chromium sulfate, chromium chloride,
Chromium oxide, chromium hydroxide and chromate, iron pigment: ferrous oxalate, iron hydroxide, barba hispanica and fervam, silicon, carbon, hydrogen；
(1) ferrochrome described in is high carbon ferro-chrome, medium carbon ferrochrome or low-carbon ferrochromium, wears into the above fine powder of 50 mesh, is put into reaction kettle,
Enough hydrochloric acid or sulfuric acid is added, 15 DEG C -120 DEG C of heating is sufficiently stirred, and reaction dissolution generates ferrochrome completely containing Cr3+、Fe2+
Solion collects hydrogen, and product new energy hydrogen is made；
(2) water is added in step (1) solution makes soluble substance become ion, contains Cr3+、Fe2+Sediment is Si in solution, is suspended
Object is C, and solution is filtered respectively, obtains filtrate and filter residue, and filter residue is washed, is separated, dry, product Si and C is made, product Si is again
Polysilicon and monocrystalline silicon are produced, filtrate is containing Cr3+、Fe2+Solution；
(3) it is added extraordinary substance in step (2) portion filtrate: alkali and Sodium Dimethyldithiocarbamate, potassium ferrocyanide, potassium ferricyanide, a kind of in oxalic acid or two
Kind or more, make Fe2+It is precipitated as FeC completely2O, fervam, barba hispanica are filtered, washed, dry, and product F eC is made2O4, fervam,
Barba hispanica, filtrate Cr3+Solution；
(4) Cr in step (3)3+Solution produces different product；
①.Cr3+Solution produces chrome tanning agent or trivalent chromium plating solution；
②.Cr3+Solution evaporation, crystallization, separation, dry obtained product chromic salt；
③.Cr3+Carbonate, bicarbonate, hydroxide, ammonium hydroxide are added in solution, makes Cr3+It is precipitated as Cr (OH) completely3, mistake
Filter, washing, crystallization, drying, are made product chromium hydroxide, and product chrome green is made in chromium hydroxide high-temperature calcination；
④.Cr3+Extraordinary reactive material: percarbonate, persulfate, hydrogen peroxide, oxygen, peroxide salt, Gao Meng is added in solution
Hydrochlorate, hypochlorite, carbonate or alkali, agitating and heating oxidation reaction make Cr in solution3+It is oxidized to Cr6+, it is molten that chromate is made
Liquid or dichromate solution；
A. by chromatedsolution or dichromate solution, evaporative crystallization is separated, dry, and product chromate or bichromate is made；
B. acid acidification or electrolysis method are added in chromatedsolution, chromatedsolution is made to generate dichromate solution, evaporation knot completely
Brilliant, separation, dry, obtained product bichromate；
(5) in step (2) portion filtrate or in step (3) portion filtrate, extraordinary reactive material: percarbonate, persulfuric acid is added
Salt, hydrogen peroxide oxygen, peroxide salt, permanganate, hypochlorite, carbonate or alkali, agitating and heating oxidation reaction make in solution
Cr3+It is oxidized to Cr6+, chromatedsolution or dichromate solution is made, makes Fe in solution2+It is precipitated as Fe (OH) completely3；
1. separates chromatedsolution or dichromate solution, evaporative crystallization, dry, product chromate or dichromic acid is made
Salt；
2. acid acidification or electrolysis method are added in chromatedsolution, chromatedsolution is made to generate dichromate solution, evaporation knot completely
Brilliant, separation, dry, obtained product bichromate；
3. Fe containing Cr VI (OH)3Middle addition acid, adds reducing agent FeSO4、Na2SO3、NaHSO3、Na2S2O5Or Na2S makes
Cr6+It is reduced to Cr3+, alkali is added and generates Fe (OH)3With Cr (OH)3Precipitating, separates, is filtered, washed, drying obtained product F e
(OH)3With Cr (OH)3。
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| CN105543506B (en) * | 2016-02-19 | 2017-06-16 | 马桂文 | A kind of method for producing high-purity metal chromium |
| CN106186067B (en) * | 2016-07-06 | 2017-11-17 | 于佳湲 | A kind of method using chromite as raw material clean manufacturing chrome green |
| CN110015689B (en) * | 2019-05-22 | 2022-06-14 | 天津鑫科清洁环保技术开发有限公司 | Production process for cleanly producing hydroxyl chromium oxide and chromium salt series products by using high-carbon ferrochrome |
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| CN101041466A (en) * | 2007-01-26 | 2007-09-26 | 湖南佳飞科技发展有限公司 | Method for producing dichromium trioxide and ferrous oxalate by carbon ferro-chrome |
| CN102583540A (en) * | 2012-03-15 | 2012-07-18 | 甘肃锦世化工有限责任公司 | Method for preparing chrome oxide black and co-producing ferrous oxalate by utilizing chrome-containing cast iron acid dissolution |
| CN103253710A (en) * | 2012-05-31 | 2013-08-21 | 唐翔 | Process for producing sodium chromate from chromite through dissolution in acid and oxidization |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101041466A (en) * | 2007-01-26 | 2007-09-26 | 湖南佳飞科技发展有限公司 | Method for producing dichromium trioxide and ferrous oxalate by carbon ferro-chrome |
| CN102583540A (en) * | 2012-03-15 | 2012-07-18 | 甘肃锦世化工有限责任公司 | Method for preparing chrome oxide black and co-producing ferrous oxalate by utilizing chrome-containing cast iron acid dissolution |
| CN103253710A (en) * | 2012-05-31 | 2013-08-21 | 唐翔 | Process for producing sodium chromate from chromite through dissolution in acid and oxidization |
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Address after: 541004 1-2-2, building 33, Guantai Crystal City, No.36, Huancheng Beier Road, Qixing District, Guilin City, Guangxi Zhuang Autonomous Region Patentee after: Tang Xiang Address before: 541001 17, building 6, building 158, No. 301, the Guangxi Zhuang Autonomous Region, Guilin, Zhongshan North Road Patentee before: Tang Xiang |