CN104743510B - Carbon ferrochrome liquid phase method manufactures new energy battery material and new energy hydrogen technique - Google Patents

Carbon ferrochrome liquid phase method manufactures new energy battery material and new energy hydrogen technique Download PDF

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CN104743510B
CN104743510B CN201310755600.4A CN201310755600A CN104743510B CN 104743510 B CN104743510 B CN 104743510B CN 201310755600 A CN201310755600 A CN 201310755600A CN 104743510 B CN104743510 B CN 104743510B
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Abstract

The present invention relates to a kind of carbon ferrochrome liquid phase method manufacture new energy battery material and new energy hydrogen technique, the invented technology is advanced, energy-conserving and environment-protective, without fire coal without HTHP, the products such as new energy, a variety of new energy battery materials, pigment and chemical industry chromic salts are disposably produced by raw material liquid phase method of ferrochrome, form a series of new high-end industrial chains, change the situation that original product purpose is single, production is simple, it greatly strengthen Enterprise International Competition, promote national industry optimization and upgrading and development, it is significant.

Description

Carbon ferrochrome liquid phase method manufactures new energy battery material and new energy hydrogen technique
Technical field
The present invention relates to a kind of carbon ferrochrome liquid phase method manufacture new energy battery material and new energy hydrogen technique, belong to Metallurgic product is the technical field that raw material produces new energy battery material and new energy.
Background technology
Due to the fast development of global economy, the demand of the energy is growing day by day.With raw materials such as coal, natural gas, oil Increasingly reduce, the need for urgent need new material new energy meets economic development.The new energy such as solar energy, Hydrogen Energy, wind energy will turn into new Development and demand.New energy needs new battery material, and new battery material mainly includes:Silicon, carbon, metal, metal oxide, The materials such as metal salt.Its production process is complicated, product is single, cost is high.
Polysilicon or amorphous silicon is typically first made in the preparation method of monocrystalline silicon, then with vertical pulling method or floating zone method from molten Bar-like single crystal silicon is grown in body.The elemental silicon of melting silicon atom in solidification is arranged in many nucleus with diamond lattice, such as Really these nucleus grow up to high preferred orientation identical crystal grain, then these crystal grain it is parallel combine just crystallize into monocrystalline silicon.
Silicon single crystal rod is the raw material for producing monocrystalline silicon piece, as domestic and international market is to the fast of monocrystalline silicon piece demand Speed increase, the market demand of silicon single crystal rod is also in the trend of rapid growth.
Monocrystalline silicon is most basic material in electronic information material, belongs to semi-conducting material class.Monocrystalline silicon has penetrated into its people Every field in economy and science and techniques of defence.
Japan, the U.S. and Germany are main silicon materials producing countries.Chinese silicon materials industry starts to walk simultaneously with Japan, but always For body, production technology level is low.
With the development of semiconductor material technology, specification and quality to silicon chip are it is also proposed that higher requirement.
Predictions in 5 years of silicon chip demand show that global 300mm silicon chips will increase to 2006 from 1.3% in 2000 21.1%.The country such as Japan and the United States, Korea Spro all started progressively expansion 300mm silicon chip yield in 1999.According to incompletely statistics, entirely Ball is built at present, there are about more than 40 bars building and plan the 300mm silicon device production lines built, is mainly distributed on the U.S. and China Taiwan Deng just there are 20 a plurality of production lines in only China Taiwan, next to that Japan and Korea S., new and Europe.
Research and develop and found the factory increasingly the increasing of cost, add existing marketing and the advantage of brand so that silicon materials industry is formed The situation of " big person is permanent big ", a small number of intensive chaebol's monopolization material markets.
Polycrystalline silicon material is to reach certain purity after being purified by raw material of industrial silicon through a series of physical-chemical reaction Electronic material, is a particularly important intermediate products in silicon product industrial chain, be manufacture silicon polished, solar cell and The primary raw material of HIGH-PURITY SILICON product, is information industry and the most basic raw material of New Energy Industry.
Polysilicon product is classified:Polysilicon can be divided into metallurgical grade (industrial silicon), solar level, electronics by purity classification Level.Metallurgical grade silicon (M6):Be silicon oxide in electric arc furnaces by carbon reduction form.It is more than 90-95% typically containing Si, up to More than 99.8%.Solar-grade silicon (SG):Purity does not have clearly defining so far between metallurgical grade silicon and electronic-grade silicon.Typically Think containing Si 99.99%-99.9999% (4~6 9).Electronic-grade silicon (EG):It is general to require to contain Si>More than 99.9999%, It is ultra-pure to reach 99.9999999%~99.999999999% (9~11 9).Its electric conductivity is between the Europe li of 10-4-1010 Rice.
Polysilicon is main, the most basic work(of semi-conductor industry, electronics and information industry, solar-energy photo-voltaic cell industry Can property material.The main raw material for being used as semiconductor, is the primary raw material for manufacturing monocrystalline silicon, can make various transistors, the pole of rectification two Pipe, controllable silicon, solar cell, integrated circuit, electronic computer chip and infrared detector etc..
Polysilicon is the raw material for the unique raw material and production solar cell for preparing monocrystalline silicon.With China's monocrystalline in recent years Silicon yield is increased with average annual 26% speed, and the demand of polysilicon is growing day by day.
Production of polysilicon technology mainly has:Improved Siemens, silane thermal decomposition process and fluidized bed process.That is researching and developing also has metallurgy The new technology of the inexpensive polysilicon of the manufacture such as method, gas-liquid sedimentation, heavily doped scrap silicon method.
85% polysilicon is produced using improved Siemens in the world, and the polysilicon of remaining method production is only accounted for 15%.Improved Siemens production technology is only introduced below.
Substantial amounts of waste water, waste liquid discharge are produced in polysilicon production process, such as:1000 tons of polysilicons of production will have trichlorine hydrogen 3500 tons of silicon, 4500 tons of waste liquids of silicon tetrachloride are produced, and the trichlorosilane and silicon tetrachloride of unprocessed recovery, which are that one kind is poisonous, to be had Evil liquid.Need to polysilicon by-product trichlorosilane, silicon tetrachloride by multistage rectification purification etc. chemical treatment, could become give up into It is precious.
Therefore, silicon materials industrial development is internationalized increasingly, grouping of the world economy, produce high concentration, promote government, research institutions, Group of enterprise and scientific research personnel, research and develop new product new method, and many new inventions, which are newly created, arises at the historic moment.Such as:" battery oxygen SiClx composite ", application number:201210130243.8, publication number:103378356A, publication date:2013-10-30;It is " a kind of The method for preparing solar cell and silicon materials ", application number:200610031434.3, publication number:1830776, publication date: 2006-09-13. the problem of these inventive methods are present:Firstth, all it is simple to produce silicon materials or by silicon materials and other materials Combination;Secondth, cost of material is high;3rd, kind atomistic competition advantage is not strong.With the development of science and technology, compound multi items Production method will turn into trend.
The content of the invention
It is an object of the invention to economize on resources, cost is reduced, intensive diversification innovation and development forms high-end product production Industry chain, promotes scientific and technological economy and social development.
The purpose of the present invention is reached by following measure:
A kind of carbon ferrochrome liquid phase method manufacture new energy battery material and new energy hydrogen technique, it is characterised in that:
1. ferrochrome is worn into fine powder, it is put into reactor, acid adding dissolving ferrochrome adds extraordinary material heating reaction, is made Product:New energy hydrogen, new energy battery material includes Prussian blue and its derivative or rattan scholar is blue and its derivative, oxalic acid are sub- Iron, silicon, carbon, chromium sulfate or chromium chloride, chromium oxide, chromium hydroxide, iron hydroxide, chromate;
2. according to ferrochrome in claim 1 be high carbon ferro-chrome, medium carbon ferrochrome or low-carbon ferrochromium wear into 50 mesh above fine powders (or Person takes carbon ferrochrome to smelt 50 mesh above fine powders of melting), it is put into reactor, addition enough hydrochloric acid or sulfuric acid, 15 DEG C of heating- 100 DEG C are sufficiently stirred for, reaction dissolving, ferrochrome is generated ion (Cr completely3+、Fe2+) solution, hydrogen is collected, the new energy of product is made Source hydrogen;
3. soluble substance is changed into ion according to water is added in claim 2 solution, containing Cr3+、Fe2+Sediment in solution For Si, suspension is C, and solution is filtered respectively, obtains filtrate and filter residue, and filter residue is scrubbed, separate, dry, be made product Si and C, product Si produce polysilicon and monocrystalline silicon again, and filtrate is containing Cr3+、Fe2+Solution and micro metal ion;
4. make Fe according to oxalic acid is added in claim 3 filtrate2+FeC is precipitated as completely2O4, filter, wash, crystallize, do It is dry, product F eC is made2O4, filtrate is Cr3+Solution and trace element, add Sodium Dimethyldithiocarbamate or sulfide, remove other micro Metal ion, Cr must be contained by filtering3+Filtrate;
5. according to potassium ferrocyanide or potassium ferricyanide is added in claim 3 filtrate, make Fe in solution2+It is precipitated as completely Prussian blue Or rattan scholar is blue, filters, wash, dry obtained product is Prussian blue or rattan scholar is blue, filtrate is Cr3+Solution;
6. according to addition potassium ferrocyanide or potassium ferricyanide and soluble-salt Cu in claim 3 filtrate2+、Zn2+、Mn2+、Co3+、Ni2 +、Y3+、Ti3+、Pb2+、Ce3+、Cs+、Cd2+、La3+、Ga3+、Bi3+、Zr4+、In3+、Sn2+One or both of more than, generation is yellow Blood salt derivative or potassium ferricyanide derivative, filtering, washing, dry obtained product potassium ferrocyanide derivative or potassium ferricyanide derivative, filter Liquid is Cr3+Solution;
7. according to Cr in claim 4,5,63+Solution produces different product;
(1).Cr3+Product chromic salt is made in solution evaporation drying;
(2).Cr3+Carbonate, bicarbonate, hydroxide, ammoniacal liquor are added in solution, makes Cr3+Cr is precipitated as completely (OH)3, filter, wash, crystallize, dry, product chromium hydroxide is made, the obtained product three of chromium hydroxide high-temperature calcination aoxidizes two Chromium:
(3).Cr3+Extraordinary reflection material is added in solution: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+It is oxidized to Cr6+, chromatedsolution (CrO is made4 2-Or bichromate is molten Liquid Cr2O7 2-
A. by chromatedsolution (CrO4 2-) or dichromate solution (Cr2O7 2-), evaporative crystallization is separated, and is dried, and production is made Product chromate or bichromate;
B. chromatedsolution (CrO4 2-) in add acid acidifying (sulfuric acid process, carbonizatin method, electrolysis) make chromatedsolution (CrO4 2-) generation dichromate solution (Cr completely2O7 2-), product bichromate is made in evaporative crystallization, separation, drying.
8. according to claim 3 filtrate Fe2+、Cr3+Extraordinary reflection material is added in solution:Percarbonate (X2CO4), over cure Hydrochlorate (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+, chromate is made Solution (CrO4 2-) or dichromate solution Cr2O7 2-, make Fe in solution2+Fe (OH) is precipitated as completely3
(1) is by chromatedsolution (CrO4 2-) or dichromate solution (Cr2O7 2-), evaporative crystallization is separated, and is dried, and is made Product chromate or bichromate;
(2) chromatedsolutions (CrO4 2-) in add acid acidifying (sulfuric acid process, carbonizatin method, electrolysis) make chromatedsolution (CrO4 2-) generation dichromate solution (Cr completely2O7 2-), product bichromate is made in evaporative crystallization, separation, drying.
(3) Fe containing Cr VI (OH)3It is middle to add acid, add reducing agent FeSO4、Na2SO3、NaHSO3、Na2S2O5、Na2S Make Cr6+It is reduced to Cr3+, add alkali generation Fe (OH)3With Cr (OH)3Precipitation, separation, filtering, washing, dry obtained product F e (OH)3With Cr (OH)3
9. according to claim 3,4,5,6,7,8 manufacture new energy battery material is Prussian blue, Prussian blue derivative, Rattan scholar indigo plant, the blue derivative of rattan scholar, ferrous oxalate, silicon, carbon, chromium sulfate or chromium chloride, chromium oxide, chromium hydroxide, are used as new energy Battery material, manufacture solar cell, battery, Hydrogen Energy battery.
In order to preferably make this inventive technique implement industrialized production as soon as possible, tried on March 18th, 2013 Test production.
Embodiment
1. high carbon ferro-chrome 1000kg is worn into 200 mesh above fine powders, it is put into reactor, adds enough sulfuric acid 3000kg, 15 DEG C -100 DEG C of heating is sufficiently stirred for, reaction dissolving, ferrochrome is generated ion (Cr completely3+、Fe2+) solution, collect Hydrogen, is made product new energy 40kg hydrogen;
Soluble substance is set to be changed into ion 2. adding water in solution, containing Cr3+、Fe2+Sediment is Si in solution, and suspension is C, solution is filtered respectively, obtains filtrate and filter residue, and filter residue is scrubbed, is separated, and is dried, and product Si is made:30kg and C:70kg, production 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+FeC is precipitated as completely2O4, filtering, washing, crystallization, dry, obtained production Product FeC2O4:1100kg, filtrate is Cr3+Solution and trace element, add Sodium Dimethyldithiocarbamate 0.05kg, remove other micro metals Ion, Cr must be contained by filtering3+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, filter, wash, crystallize, do It is dry, product chromium hydroxide is made:Product chrome green is made in 420kg, chromium hydroxide high-temperature calcination:310kg;
(3).Cr3+Extraordinary reflection material 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, dried, and product sodium chromate 350kg. is made
5. new energy hydrogen 40kg, new energy battery material are produced according to process above:Ferrous oxalate 1100kg, silicon 30kg, carbon 70kg, chromium sulfate 1500kg, chromium oxide 310kg, chromium hydroxide 420kg, as new energy battery material, manufacture is too Positive energy battery, battery, Hydrogen Energy battery.
It facts have proved that the invented technology is advanced, energy-conserving and environment-protective, without fire coal without HTHP, using ferrochrome as raw material liquid phase Method disposably produces the products such as new energy, a variety of new energy battery materials, pigment and chemical industry chromic salts, forms a series of new height Industrial chain is held, the situation that original product purpose is single, production is simple is changed, greatly strengthen Enterprise International Competition, promote Enter national industry optimization and upgrading and development, it is significant.

Claims (1)

1. a kind of carbon ferrochrome liquid phase method manufacture new energy battery material and new energy hydrogen technique, it is characterised in that:By ferrochrome Fine powder is worn into, is put into reactor, acid adding dissolving ferrochrome adds extraordinary material heating reaction, product is made:New energy hydrogen, New energy battery material includes Prussian blue or rattan scholar indigo plant, ferrous oxalate, silicon, carbon, chromium sulfate or chromium chloride, chromium oxide, hydrogen-oxygen Change chromium, iron hydroxide, chromate;
(1) ferrochrome described in is high carbon ferro-chrome, medium carbon ferrochrome or low-carbon ferrochromium, wears into 50 mesh above fine powders, is put into reactor, Enough hydrochloric acid or sulfuric acid is added, 15 DEG C -100 DEG C of heating is sufficiently stirred for, reaction dissolving makes ferrochrome generate Cr completely3+、Fe2+From Sub- solution, collects hydrogen, and product new energy hydrogen is made;
(2) water is added in steps (1) solution makes soluble substance be changed into ion, containing Cr3+、Fe2+Sediment is Si in solution, is suspended Thing is C, and solution is filtered respectively, obtains filtrate and filter residue, and filter residue is scrubbed, is separated, and is dried, and product Si and C is made, product Si is again Polysilicon and monocrystalline silicon are produced, filtrate is containing Cr3+、Fe2+And micro metal ion solution;
(3) oxalic acid is added in steps (2) portion filtrate makes Fe2+FeC is precipitated as completely2O4, filtering, washing, crystallization, dry, system Obtain product F eC2O4, filtrate is Cr3+And trace element solution, Sodium Dimethyldithiocarbamate or sulfide are added, other micro metals are removed Ion, Cr must be contained by filtering3+Filtrate;
(4) potassium ferrocyanide or potassium ferricyanide are added in steps (2) portion filtrate, makes Fe in solution2+Prussian blue or rattan is precipitated as completely Scholar is blue, filters, washs, dry obtained product is Prussian blue or rattan scholar is blue, filtrate is Cr3+Solution;
(5) potassium ferrocyanide or potassium ferricyanide and soluble-salt Cu are added in steps (2) portion filtrate2+、Zn2+、Mn2+、Co3+、Ni2+、Y3 +、Ti3+、Pb2+、Ce3+、Cs+、Cd2+、La3+、Ga3+、Bi3+、Zr4+、In3+、Sn2+One or both of more than, generate potassium ferrocyanide Derivative or potassium ferricyanide derivative, filter, wash, drying obtained product potassium ferrocyanide derivative or potassium ferricyanide derivative, filtrate is Cr3+Solution;
(6) is by Cr in step (3), (4), (5)3+Solution produces different product;
1. parts Cr3+Product chromic salt is made in solution evaporation drying;
2. parts Cr3+Carbonate, bicarbonate, hydroxide, ammoniacal liquor are added in solution, makes Cr3+Cr (OH) is precipitated as completely3, Filter, wash, crystallize, dry, product chromium hydroxide, the obtained product chrome green of chromium hydroxide high-temperature calcination is made;
3. parts Cr3+Extraordinary reactive material is added in solution:Percarbonate, persulfate, hydrogen peroxide, oxygen, peroxide salt, Permanganate, hypochlorite, carbonate, alkali, agitating and heating oxidation reaction make Cr in solution3+It is oxidized to Cr6+, chromate is made Solution or dichromate solution;
A. by chromatedsolution or dichromate solution, evaporative crystallization is separated, and is dried, and product chromate or bichromate is made;
B. acid acidifying is added in chromatedsolution makes chromatedsolution generate dichromate solution completely, evaporative crystallization, separation, does It is dry, product bichromate is made;
(7) part steps (2) contain Fe2+、Cr3+Extraordinary reactive material is added in Filtrate solutions:Percarbonate, persulfate, dioxygen Water, oxygen, peroxide salt, permanganate, hypochlorite, carbonate, alkali, agitating and heating oxidation reaction make Cr in solution3+Oxidation For Cr6+, chromatedsolution or dichromate solution is made, makes Fe in solution2+Fe (OH) is precipitated as completely3
1. is by chromatedsolution or dichromate solution, and evaporative crystallization is separated, dried, and product chromate or dichromic acid is made Salt;
2. acid acidifying is added in chromatedsolutions makes chromatedsolution generate dichromate solution completely, evaporative crystallization, separation, Dry, product bichromate is made;
3. Fe containing Cr VI (OH)3It is middle to add acid, add reducing agent FeSO4、Na2SO3、NaHSO3、Na2S2O5, Na2S, make Cr6+It is reduced to Cr3+, add alkali generation Fe (OH)3With Cr (OH)3Precipitation, separation, filtering, washing, dry obtained product F e (OH)3With Cr (OH)3
(8) Prussian blue, the rattan scholar indigo plant, ferrous oxalate, silicon, carbon, chromium sulfate or the chromium chloride that are obtained in above-mentioned steps, chromium oxide, Chromium hydroxide is used as new energy battery material, manufacture solar cell, battery, Hydrogen Energy battery.
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CN107236967A (en) * 2016-03-28 2017-10-10 唐翔 The preparation method of high-purity refractory metal and device

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