CN106315675B - A kind of method that utilization tanned wastes chromium mud produces chromium sulfate basic - Google Patents
A kind of method that utilization tanned wastes chromium mud produces chromium sulfate basic Download PDFInfo
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- CN106315675B CN106315675B CN201610707456.0A CN201610707456A CN106315675B CN 106315675 B CN106315675 B CN 106315675B CN 201610707456 A CN201610707456 A CN 201610707456A CN 106315675 B CN106315675 B CN 106315675B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/08—Chromium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
- C01G37/033—Chromium trioxide; Chromic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method that utilization tanned wastes chromium mud produces chromium sulfate basic.Waste material chromium mud is subjected to air dry, drying first, the chromium mud after drying and sodium hydroxide are mixed and are placed in rotary kiln, and adds oxidant is calcined；Material after roasting carries out water circulation filtering and washing, removes impurity and obtains chromium acid sodium solution；Sulfuric acid is added in resulting solution and carries out the obtained sodium dichromate of reaction, sulfuric acid is continuously added and is reacted, and be slowly added to after sucrose, reaction obtain liquid chromium sulfate basic；Finally chromium sulfate basic solution is dried, powdery chromium sulfate basic is obtained.Technical solution of the present invention takes full advantage of waste material chromium mud, turns waste into wealth, recycles, has saved resource and the energy.Curriery pollution of chromium is not only solved the problems, such as, while process hides cost can also be reduced.While pollution of chromium is solved, the economic benefit and social benefit of enterprise are also improved significantly.
Description
First, technical field：
The present invention relates to a kind of preparation method of chromium sulfate basic, and in particular to one kind utilizes tanned wastes chromium mud production alkali
The method of formula chromium sulfate.
2nd, background technology：
Chrome tanning is a crucial process in leather making processes, because in tannery, chromium is not fine by collagen
Dimension is fully absorbed, and the utilization rate of Chrome Tanning Liquor only has 70% or so, and remaining 30% or so Chrome Tanning Liquor is not utilized and entered
In waste water, severe contamination is on the one hand caused to environment, significant wastage also on the other hand is caused to resource.
At present, the processing most common method of Chrome Tanning Wastewater is alkaline chemical precipitation method, i.e., a certain amount of alkalescence will be added in waste liquid
Material, makes chromium ion formation chromium hydroxide, and it is that (active ingredient is three oxidations two to chromium mud in chromium mud to be then filtrated to get precipitation
Chromium).
Chromium sulfate basic is indispensable tanning agent in curriery, and it plays the part of weight during leather is changed into from rawhide
The role wanted.Rawhide is exactly leather after tanning, and weatherability and corrosion resistance are significantly improved.At present, process hides company is mostly
Being just discharged into big small river after tanning solution (composition is chromium sulfate) simple process, or turned into alkali and lime neutralisation of sulphuric acid chromium
Chromium hydroxide, these chromium mud storage warehouse or transfer stock, thus bring pollution to environment, pressure are brought to society
Power.Therefore, it is badly in need of a kind of technology of effective processing waste material chromium mud of research and development.
3rd, the content of the invention：
The technical problem to be solved in the present invention is：Fail to be effectively addressed according to current waste material chromium mud and pollute ring
Border, the technical barrier for wasting the energy, the present invention provide a kind of method that utilization tanned wastes chromium mud produces chromium sulfate basic.Pass through
Technical solution of the present invention, can effectively utilize waste material chromium mud, so as to solve environmental pollution, the technology of the waste energy that chromium mud is caused
Problem.
In order to solve the above problems, the technical scheme that the present invention takes is：
The present invention provides a kind of method that utilization tanned wastes chromium mud produces chromium sulfate basic, the production method include with
Lower step：
A, the weight/mass percentage composition that tanned wastes chromium mud is carried out chromium mud reclaimed water after air dry, air dry first are 30~40%；
Then (waste heat produced using roasting) is dried, and the weight/mass percentage composition of gained chromium mud reclaimed water is 5~10% after drying；
B, step a dried after chromium mud be well mixed with sodium hydroxide, chromium mud and sodium hydroxide are therebetween
Weight ratio is 1:30~35, batch (-type) rotary kiln is put into after mixing, and oxidant sodium nitrate is added, the addition of sodium nitrate accounts for baking
The 3~5% of chromium mud weight, are then heated after dry；500~600 DEG C are heated to through 3~5h first to be calcined,
1~2h is incubated under this temperature conditions, roasting is cooled to 100~200 DEG C after terminating；
C, by step b be calcined after material put into metal trough in, and through 3~5 times addition water circulation suction filtrations, remove material in it is miscellaneous
Matter calcium oxide, aluminum oxide and iron oxide, obtain the chromium acid sodium solution that Baume degrees is 30~40；
In d, reactor of the chromium acid sodium solution input with agitator for obtaining step c, start and stir and add sulfuric acid
Acidification reaction is carried out, reaction temperature is 50~80 DEG C；Sodium chromate is in terms of sterling, sulfuric acid in terms of 100%, the sodium chromate and sulfuric acid
The ratio of the two addition is 1 ton：200~300 kilograms；After testing, the reaction knot when the pH value of reaction solution is 2.5~2.8
Beam, obtains sodium dichromate solution；Sulfuric acid is continuously added to be reacted, sodium dichromate is in terms of sterling, sulfuric acid in terms of 100%, weight chromium
Sour sodium is 1 with the weight ratio of sulfuric acid therebetween:0.95~0.98；Sucrose is slowly added under constant agitation to carry out instead
Should, sucrose is in terms of 100%, sodium dichromate in terms of sterling, addition weight ratio between sodium dichromate and sucrose is 1:0.1~
0.145；After testing, react and terminate when the Cr VI in reaction solution is fully converted to trivalent chromium, it is 33~42 to obtain basicity
Liquid chromium sulfate basic；
E, chromium sulfate basic solution obtained by step d is dried, obtain chrome green weight/mass percentage composition for 21~
25% powdery chromium sulfate basic.
The method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, tanned wastes chromium described in step a
The weight/mass percentage composition of mud reclaimed water is 75~85%, and the weight/mass percentage composition of chrome green is 5~8%.
The method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, sodium hydroxide described in step b
Weight/mass percentage composition is 60~98%；The sodium nitrate is industrial goods, and its weight/mass percentage composition is 98%.
The method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, described in step c and through 3~5 times
Water circulation suction filtration is added, the addition of its reclaimed water is 1~1.2 times of material.
The method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, the quality of sulfuric acid described in step d
Percentage composition is 93%.
Gained liquid base formula sulphur in the method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, step d
The Baume degrees of sour chromium is that the weight/mass percentage composition of chrome green in 40~50, liquid chromium sulfate basic is 10~12%.
Drying in the method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, step e uses roller
Dry or be spray-dried.
During the method that chromium sulfate basic is produced according to above-mentioned utilization tanned wastes chromium mud, the roller drying, rolling
0.3~0.4mpa steam is passed through in cylinder, drying temperature is 70~80 DEG C；In the spray-drying process, inlet temperature of stabilizer is controlled
For 90~120 DEG C.
The present invention produces the chromium sulfate basic of other basicity if desired, the gained liquid base formula sulfuric acid in above-mentioned steps d
Technical grade sodium carbonate is added in chromium or thenardite is adjusted, the chromium sulfate basic of basicity needed for obtaining.
The positive beneficial effect of the present invention：
1st, liquid sodium chromate is made in waste material chromium mud (utilizing chromium hydroxide therein) and alkali by technical solution of the present invention, then is used
Sodium chromate and sulfuric acid reaction, chromium sulfate basic is made with sucrose reduction.Technical solution of the present invention takes full advantage of waste material chromium mud, becomes
Waste be changed into values, recycles, and has saved resource and the energy.Curriery pollution of chromium is not only solved the problems, such as, while system can also be reduced
Remove from office cost.While pollution of chromium is solved, the economic benefit and social benefit of enterprise are also improved significantly.
2nd, the chromium sulfate basic prepared using technical solution of the present invention, its basicity is 33~42, chrome green
Weight/mass percentage composition is 21~25%, is the important tanning agent of curriery, solves the chrome wastewater pollution problem of curriery, real real
Having showed turns waste into wealth, and recycles, with significant economic benefit and social benefit.
3rd, by technical solution of the present invention, chromic oxide content can be prepared from low content to high content by adjustment
Chromium sulfate basic, and content is easily controlled, the alkali formula sulfuric acid steady quality of production, overcomes and the production of chromium mud is directly dissolved with sulfuric acid
The shortcoming of chromium sulfate basic.
4th, embodiment：
The present invention is expanded on further with reference to embodiments, but is not intended to limit present disclosure.
The weight/mass percentage composition for the tanned wastes chromium mud reclaimed water that the present invention is used is 75~85%, the quality of chrome green
Percentage composition is 5~8%.
Embodiment 1：
The method that the present invention produces chromium sulfate basic using tanned wastes chromium mud, the detailed step of the production method is as follows：
A, the weight/mass percentage composition that tanned wastes chromium mud is carried out chromium mud reclaimed water after air dry, air dry first are 36%；Then
(waste heat produced using roasting process is dried) is dried, the weight/mass percentage composition of gained chromium mud reclaimed water is after drying
8%；
B, step a is dried after chromium mud and sodium hydroxide (weight/mass percentage composition of sodium hydroxide is 80%) mixed
Uniformly, the weight ratio of chromium mud and sodium hydroxide therebetween is 1:33, batch (-type) rotary kiln is put into after mixing, and add oxidant
(sodium nitrate is industrial goods to sodium nitrate, and its weight/mass percentage composition is 98%), the addition of sodium nitrate accounts for chromium mud weight after drying
4%, then heated；550 DEG C are heated to through 4h first to be calcined, 1.5h is incubated under this temperature conditions, be calcined
160 DEG C are cooled to after end；
C, step b is calcined after material put into metal trough, and through 4 times add water circulation suction filtrations (addition of water be thing
1.1 times of material), oxidation of impurities calcium, aluminum oxide and iron oxide in material are removed, the chromium acid sodium solution that Baume degrees is 37 is obtained；
In d, reactor of the chromium acid sodium solution input with agitator for obtaining step c, start and stir and add sulfuric acid
Acidification reaction (weight/mass percentage composition of sulfuric acid is 93%) is carried out, reaction temperature is 70 ± 5 DEG C；Sodium chromate is in terms of sterling, sulfuric acid
In terms of 100%, the ratio of both the sodium chromate and sulfuric acid addition is 1 ton：260 kilograms；After testing, as the pH of reaction solution
Be worth for 2.6 when reaction terminate, obtain sodium dichromate solution；Continuously add sulfuric acid and reacted that (weight/mass percentage composition of sulfuric acid is
93%), sodium dichromate in terms of sterling, sulfuric acid in terms of 100%, sodium dichromate and the weight ratio of sulfuric acid therebetween are 1:0.96；
Sucrose is slowly added under constant agitation to be reacted, sucrose is in terms of 100%, sodium dichromate in terms of sterling, sodium dichromate
Addition weight ratio between sucrose is 1:0.142；After testing, when the Cr VI in reaction solution is fully converted to trivalent chromium
Reaction terminates, and obtaining the liquid chromium sulfate basic that basicity is 34, (Baume degrees of gained liquid chromium sulfate basic is 44, liquid base formula
11%) weight/mass percentage composition of chrome green is in chromium sulfate；
E, chromium sulfate basic solution obtained by step d is dried (during using roller drying mode, roller drying,
0.3~0.4mpa steam is passed through in roller, drying temperature is 70~80 DEG C), obtaining chrome green weight/mass percentage composition is
23% powdery chromium sulfate basic.
Embodiment 2：
The method that the present invention produces chromium sulfate basic using tanned wastes chromium mud, the detailed step of the production method is as follows：
A, the weight/mass percentage composition that tanned wastes chromium mud is carried out chromium mud reclaimed water after air dry, air dry first are 30%；Then
(waste heat produced using roasting process is dried) is dried, the weight/mass percentage composition of gained chromium mud reclaimed water is after drying
5%；
B, step a is dried after chromium mud and sodium hydroxide (weight/mass percentage composition of sodium hydroxide is 60%) mixed
Uniformly, the weight ratio of chromium mud and sodium hydroxide therebetween is 1:35, batch (-type) rotary kiln is put into after mixing, and add oxidant
(sodium nitrate is industrial goods to sodium nitrate, and its weight/mass percentage composition is 98%), the addition of sodium nitrate accounts for chromium mud weight after drying
3%, then heated；500 DEG C are heated to through 3h to be calcined, 2h, roasting knot are incubated under this temperature conditions first
120 DEG C are cooled to after beam；
C, step b is calcined after material put into metal trough, and through 3 times add water circulation suction filtrations (addition of water be thing
1.2 times of material), oxidation of impurities calcium, aluminum oxide and iron oxide in material are removed, the chromium acid sodium solution that Baume degrees is 30 is obtained；
In d, reactor of the chromium acid sodium solution input with agitator for obtaining step c, start and stir and add sulfuric acid
Acidification reaction (weight/mass percentage composition of sulfuric acid is 93%) is carried out, reaction temperature is 60 ± 5 DEG C；Sodium chromate is in terms of sterling, sulfuric acid
In terms of 100%, the ratio of both the sodium chromate and sulfuric acid addition is 1 ton：200 kilograms；After testing, as the pH of reaction solution
Be worth for 2.5 when reaction terminate, obtain sodium dichromate solution；Continuously add sulfuric acid and reacted that (weight/mass percentage composition of sulfuric acid is
93%), sodium dichromate in terms of sterling, sulfuric acid in terms of 100%, sodium dichromate and the weight ratio of sulfuric acid therebetween are 1:0.95；
Sucrose is slowly added under constant agitation to be reacted, sucrose is in terms of 100%, sodium dichromate in terms of sterling, sodium dichromate
Addition weight ratio between sucrose is 1:0.140；After testing, when the Cr VI in reaction solution is fully converted to trivalent chromium
Reaction terminates, and obtaining the liquid chromium sulfate basic that basicity is 33, (Baume degrees of gained liquid chromium sulfate basic is 40, liquid base formula
10%) weight/mass percentage composition of chrome green is in chromium sulfate；
E, chromium sulfate basic solution obtained by step d is dried (during using roller drying mode, roller drying,
0.3~0.4mpa steam is passed through in roller, drying temperature is 70~80 DEG C), obtaining chrome green weight/mass percentage composition is
21% powdery chromium sulfate basic.
Embodiment 3：
The method that the present invention produces chromium sulfate basic using tanned wastes chromium mud, the detailed step of the production method is as follows：
A, the weight/mass percentage composition that tanned wastes chromium mud is carried out chromium mud reclaimed water after air dry, air dry first are 40%；Then
(waste heat produced using roasting process is dried) is dried, the weight/mass percentage composition of gained chromium mud reclaimed water is after drying
10%；
B, step a is dried after chromium mud and sodium hydroxide (weight/mass percentage composition of sodium hydroxide is 98%) mixed
Uniformly, the weight ratio of chromium mud and sodium hydroxide therebetween is 1:30, batch (-type) rotary kiln is put into after mixing, and add oxidant
(sodium nitrate is industrial goods to sodium nitrate, and its weight/mass percentage composition is 98%), the addition of sodium nitrate accounts for chromium mud weight after drying
5%, then heated；600 DEG C are heated to through 5h first to be calcined, 1.0h is incubated under this temperature conditions, be calcined
200 DEG C are cooled to after end；
C, step b is calcined after material put into metal trough, and through 5 times add water circulation suction filtrations (addition of water be thing
1.0 times of material), oxidation of impurities calcium, aluminum oxide and iron oxide in material are removed, the chromium acid sodium solution that Baume degrees is 40 is obtained；
In d, reactor of the chromium acid sodium solution input with agitator for obtaining step c, start and stir and add sulfuric acid
Acidification reaction (weight/mass percentage composition of sulfuric acid is 93%) is carried out, reaction temperature is 75 ± 5 DEG C；Sodium chromate is in terms of sterling, sulfuric acid
In terms of 100%, the ratio of both the sodium chromate and sulfuric acid addition is 1 ton：300 kilograms；After testing, as the pH of reaction solution
Be worth for 2.8 when reaction terminate, obtain sodium dichromate solution；Continuously add sulfuric acid and reacted that (weight/mass percentage composition of sulfuric acid is
93%), sodium dichromate in terms of sterling, sulfuric acid in terms of 100%, sodium dichromate and the weight ratio of sulfuric acid therebetween are 1:0.98；
Sucrose is slowly added under constant agitation to be reacted, sucrose is in terms of 100%, sodium dichromate in terms of sterling, sodium dichromate
Addition weight ratio between sucrose is 1:0.144；After testing, when the Cr VI in reaction solution is fully converted to trivalent chromium
Reaction terminates, and obtaining the liquid chromium sulfate basic that basicity is 42, (Baume degrees of gained liquid chromium sulfate basic is 50, liquid base formula
12%) weight/mass percentage composition of chrome green is in chromium sulfate；
E, chromium sulfate basic solution obtained by step d is dried (during using roller drying mode, roller drying,
0.3~0.4mpa steam is passed through in roller, drying temperature is 70~80 DEG C), obtaining chrome green weight/mass percentage composition is
25% powdery chromium sulfate basic.
Claims (8)
1. a kind of method that utilization tanned wastes chromium mud produces chromium sulfate basic, it is characterised in that the production method include with
Lower step：
A, the weight/mass percentage composition that tanned wastes chromium mud is carried out chromium mud reclaimed water after air dry, air dry first are 30~40%；Then
Dried, the weight/mass percentage composition of gained chromium mud reclaimed water is 5~10% after drying；
B, by step a dry after chromium mud be well mixed with sodium hydroxide, the weight of chromium mud and sodium hydroxide therebetween
Than for 1:30~35, batch (-type) rotary kiln is put into after mixing, and oxidant sodium nitrate is added, the addition of sodium nitrate is accounted for after drying
The 3~5% of chromium mud weight, are then heated；500~600 DEG C are heated to through 3~5h first to be calcined, it is warm herein
1~2h is incubated under the conditions of degree, roasting is cooled to 100~200 DEG C after terminating；
C, by step b be calcined after material put into metal trough in, and through 3~5 times addition water circulation suction filtrations, remove material in impurity oxygen
Change calcium, aluminum oxide and iron oxide, obtain the chromium acid sodium solution that Baume degrees is 30~40；
In d, reactor of the chromium acid sodium solution input with agitator for obtaining step c, start and stir and add sulfuric acid progress
Acidification reaction, reaction temperature is 50~80 DEG C；Sodium chromate is in terms of sterling, sulfuric acid in terms of 100%, the sodium chromate and both sulfuric acid
The ratio of addition is 1 ton：200~300 kilograms；After testing, when the pH value of reaction solution is 2.5~2.8, reaction terminates, and obtains
To sodium dichromate solution；Sulfuric acid is continuously added to be reacted, sodium dichromate is in terms of sterling, sulfuric acid in terms of 100%, sodium dichromate with
The weight ratio of sulfuric acid therebetween is 1:0.95~0.98；It is slowly added to sucrose under constant agitation to be reacted, sucrose
In terms of 100%, sodium dichromate in terms of sterling, addition weight ratio between sodium dichromate and sucrose is 1:0.1~0.145；Through inspection
Survey, react and terminate when the Cr VI in reaction solution is fully converted to trivalent chromium, obtain the liquid that basicity is 33%~42%
Chromium sulfate basic；
E, chromium sulfate basic solution obtained by step d is dried, it is 21~25% to obtain chrome green weight/mass percentage composition
Powdery chromium sulfate basic.
2. the method that utilization tanned wastes chromium mud according to claim 1 produces chromium sulfate basic, it is characterised in that：Step
The weight/mass percentage composition of the mud reclaimed water of tanned wastes chromium described in a is 75~85%, the weight/mass percentage composition of chrome green for 5~
8%.
3. the method that utilization tanned wastes chromium mud according to claim 1 produces chromium sulfate basic, it is characterised in that：Step
The weight/mass percentage composition of sodium hydroxide described in b is 60~98%；The sodium nitrate is industrial goods, and its weight/mass percentage composition is
98%.
4. the method that utilization tanned wastes chromium mud according to claim 1 produces chromium sulfate basic, it is characterised in that：Step
Described in c and through 3~5 addition water circulation suction filtrations, the addition of its reclaimed water is 1~1.2 times of material.
5. the method that utilization tanned wastes chromium mud according to claim 1 produces chromium sulfate basic, it is characterised in that：Step
The weight/mass percentage composition of sulfuric acid described in d is 93%.
6. the method that utilization tanned wastes chromium mud according to claim 1 produces chromium sulfate basic, it is characterised in that：Step
The Baume degrees of liquid chromium sulfate basic obtained by d is that the quality percentage of chrome green in 40~50, liquid chromium sulfate basic contains
Measure as 10~12%.
7. the method that utilization tanned wastes chromium mud according to claim 1 produces chromium sulfate basic, it is characterised in that：Step
Drying in e uses roller drying or spray drying.
8. the method that utilization tanned wastes chromium mud according to claim 7 produces chromium sulfate basic, it is characterised in that：It is described
0.3~0.4mpa steam is passed through during roller drying, in roller, drying temperature is 70~80 DEG C；It is described spray dried
Cheng Zhong, it is 90~120 DEG C to control inlet temperature of stabilizer.
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| CN109433781A (en) * | 2018-09-19 | 2019-03-08 | 河北赢丰再生资源利用有限公司 | A kind of recycling and harmless treatment process of the circulating waste garrulous material of leather containing chromium |
| CN109384260A (en) * | 2018-12-14 | 2019-02-26 | 宁波欣辉环保科技有限公司 | A kind of technique that electroplating sludge extracts chromium sulfate basic |
| CN112916589A (en) * | 2021-02-26 | 2021-06-08 | 丁吉东 | Method for treating chromium-containing waste in leather tanning |
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| CN101723459A (en) * | 2008-10-27 | 2010-06-09 | 张晓东 | Method for manufacturing ceramic pigment chrome green from waste materials of chromium salt factory |
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