CN102115105A - Production method of alum - Google Patents

Production method of alum Download PDF

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Publication number
CN102115105A
CN102115105A CN 201110023110 CN201110023110A CN102115105A CN 102115105 A CN102115105 A CN 102115105A CN 201110023110 CN201110023110 CN 201110023110 CN 201110023110 A CN201110023110 A CN 201110023110A CN 102115105 A CN102115105 A CN 102115105A
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China
Prior art keywords
alum
coal
coal gangue
reaction
bone
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CN 201110023110
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Chinese (zh)
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张伟峰
彭小艳
姜桂生
彭清
彭海泉
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WANZAI JINZHOU CHEMICAL FACTORY
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WANZAI JINZHOU CHEMICAL FACTORY
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Priority to CN 201110023110 priority Critical patent/CN102115105A/en
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Abstract

The invention is to provide a production method of alum, which uses coal gangue and/or stone coal as a raw material, and comprises the following steps: A) immersing the coal gangue and/or stone coal in sulfuric acid solution to obtain solid and liquid mixed solution containing alum; B) separating by filtering to obtain the mixed solution, and removing slag; and C) standing the separated solution for settling. In the invention, the conventional roasting method is not used, soot and waste gas emission is avoided, and the production cost and equipment investment are low.

Description

The production method of alum
Technical field: the production method that the present invention relates to a kind of alum.
Background technology: alum is a kind of important chemical feedstocks, it is meant that mainly potassium alum is a potassium aluminium sulfate, one is to carry out a word used in place name with alunite or the mine tailing that contains alunite to fire and be equipped with, as Chinese patent application number is that 03112613.8 " production method of crystal alum " and application number are that 201010115907.4 " a kind of chloridizing roasting method of material containing alunite " all is to adopt alunite or alunite mine tailing are carried out roasting earlier, and then carries out chemical treatment; Produce a large amount of waste gas during because of roasting atmospheric environment is produced bigger pollution, after burning, also produce a large amount of waste residues simultaneously; Exhaust gas discharged and waste residue still can cause certain pollution to environment; And production cost rises, and facility investment is big.
Summary of the invention: the present invention is exactly the production method that a kind of alum will be provided, and it is to be that raw material does not use traditional roasting method with colliery depleted coal gangue or bone coal, no flue dust exhaust gas emission, and production cost is low, and facility investment is little.Technical scheme of the present invention is to be raw material with coal gangue and/or bone coal, and described method comprises:
A) with sulphuric acid soln stain coal gangue and/or bone coal, obtain aluminated solid, liquid mixing solutions;
B) the described mixing solutions of filtering separation, slagging-off; With
C) separation solution is staticly settled.
The production method of alum of the present invention is to carry out as follows:
A) described sulphuric acid soln dipping coal gangue and/or bone coal, its sulphuric acid soln concentration is 20-98wt%, add additive simultaneously and account for coal gangue/or bone coal mass ratio 0.5-1.5% oxymuriate or villaumite, the control coal gangue/or bone coal: sulfuric acid: quality is than=1: 0.2-0.5: 0.1-0.15, and mix, flood 100-200h down in normal temperature and get reaction mass;
B) in A) step reaction mass in add entry, controlling described reaction mass and quality ratio is 1: 1-2; Add 40-85 ℃ of thermal control dipping temperature of reaction, reaction times 20-90min gets the solid, liquid mixed solution, and filter cleaner gets filtrate;
C) filtrate is staticly settled system alum.
The present invention preferably is broken to the 20-120 order with described coal gangue and/or stone coal powder.
Oxymuriate of the present invention is sodium chlorate or Potcrate, preferred sodium chlorate, and villaumite is sodium-chlor or Repone K.
The present invention is 10-36h the control time of staticly settling.
Filtration of the present invention adopts plate-and-frame filter press to filter.
The present invention controls described dipping temperature of reaction at 50-60 ℃.
The selected raw material of the present invention is a bone coal, preferred coal gangue.
The present invention with low-calorie coal gangue or bone coal as raw materials for production, do not need raw materials for production are carried out roasting, therefore can not produce poisonous, noxious gas emission, can not pollute atmospheric environment, adopt simultaneously cycle production process in process of production, waste residue can be used as the building materials raw material, can carry out the circulation comprehensive utilization to resource, is the low-carbon environment-friendly production method.
Utilizing the inventive method is that the alum product of raw material production detects through quality of chemical products supervision and inspection station, Hunan Province that every quality index all reaches and the requirement that is above standard with coal gangue or bone coal, and assay sees Table 1
Censorship unit: Jin Zhou chemical plant, Wanzai County
Sample size: 100g; Kind of inspection: supervision and inspection
Sample size: 6000kg; Sample state: crystal
The every quality index of table 1 potassium aluminium sulfate (alum) product
Interventions Requested Standard value % Measured value Conclusion
Potassium aluminium sulfate KAl (SO 4) 2.12H 2O ≥97.6 ?99.78 Qualified
Iron (Fe) ≤0.05 ?0.0064 Qualified
Heavy metal (Pb) ≤0.005 ?0.0001 Qualified
Arsenic (As) ≤0.001 ?<0.00005 Qualified
Water-insoluble ≤0.2 ?0.001 Qualified
Moisture ≤1.0 ?0.02 Qualified
The inventive method technological process of production is as follows:
Coal gangue, bone coal → pulverizing+sulfuric acid → stirring reaction → press filtration, filtration → precipitate and separate → product.
The main chemical equation that the present invention relates to:
K 2O+H 2SO 4→K 2SO 4+H 2O
Al 2O 3+3H 2SO 4→Al 2(SO 4) 3+3H 2O
K 2SO 4+Al 2(SO 4) 3+24H 2O→2KAl(SO 4) 2.12H 2O?↓
The system alumen exsiccatum
Figure BDA0000044683690000021
Embodiment: the present invention is elaborated below in conjunction with embodiment:
Embodiment 1
Colliery powder is broken to particle diameter crosses the 60-80 mesh sieve, place reaction vessel, adding the concentration that accounts for coal gangue weight 25% is 90% sulphuric acid soln, account for coal gangue respectively and weigh 10% and 1% water and additive sodium chlorate, fully mix, reacted 120 hours down in normal temperature, make reaction material, in reaction material, add the water that accounts for 1.5 times of amounts of reaction material quality then, again it is carried out heat temperature raising to 50-80 ℃ of reaction 60 minutes, make solid, the liquid mixing solutions, to consolidate, the liquid mixing solutions carries out filtering separation with plate-and-frame filter press and removes filter residue, and filter residue reclaims and is used to prepare material of construction, as cement, common brick etc., filtrate being contains the solution left standstill 24 hours of potassium alum, precipitates and isolates solid potassium alum KAl (SO 4) 2.12H 2O, the filtrate that precipitates and isolates continuation is reclaimed and returns use, to KAl (SO 4) 2.12H 2O heats to anhydrate and promptly prepares solid alum KAl (SO 4) 2Product.
Embodiment 2 all the other method stepss except that following explanation are identical with example 1;
With the bone coal is raw material, stone coal powder is broken to particle diameter crosses the 60-80 mesh sieve, places reaction vessel to add additive Potcrate or the Repone K that accounts for bone coal weight 1%, and controlling quality is than being bone coal: sulfuric acid: water=1: 0.4: 0.12, sulphuric acid soln concentration are 50%.

Claims (9)

1. the production method of an alum is characterized in that with coal gangue and/or bone coal be raw material, and described method comprises:
A) with sulphuric acid soln stain coal gangue and/or bone coal, obtain aluminated solid, liquid mixing solutions;
B) the described mixing solutions of filtering separation, slagging-off; With
C) separation solution is staticly settled.
2. according to the production method of the described alum of claim 1, it is characterized in that described method carries out as follows:
A) described sulphuric acid soln dipping coal gangue and/or bone coal, its sulphuric acid soln concentration is 20-98wt%, add additive simultaneously and account for coal gangue/or bone coal mass ratio 0.5-1.5% oxymuriate or villaumite, the control coal gangue/or bone coal: sulfuric acid: quality ratio=1:0.2-0.5:0.1-0.15, and mix, flood 100-200h down in normal temperature and get reaction mass;
B) in A) add entry in the reaction mass in step, control described reaction mass and quality than for 1:1-2; Add 40-85 ℃ of thermal control dipping temperature of reaction, reaction times 20-90min gets the solid, liquid mixed solution, and filter cleaner gets filtrate;
C) filtrate is staticly settled system alum.
3. according to the method for claim 1 or 2 described alum, it is characterized in that described coal gangue and/or stone coal powder are broken to the 20-120 order.
4. according to the method for the described alum of claim 2, it is characterized in that described oxymuriate is sodium chlorate or Potcrate, villaumite is sodium-chlor or Repone K.
5. according to the method for claim 1 or 2 described alum, it is characterized in that the control time of staticly settling is 10-36h.
6. according to the method for claim 1 or 2 described alum, it is characterized in that described filtration employing plate-and-frame filter press filters.
7. according to the method for the described alum of claim 2, it is characterized in that controlling described dipping temperature of reaction at 50-60 ℃.
8. according to the method for the described alum of claim 1, it is characterized in that described raw material is a bone coal.
9. according to the method for the described alum of claim 1, it is characterized in that described raw material is a coal gangue.
CN 201110023110 2011-01-21 2011-01-21 Production method of alum Pending CN102115105A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445331A (en) * 2014-12-16 2015-03-25 兴安宸亿工贸有限公司 Method for using wastewater and waste residues generated in alum production process
CN105271340A (en) * 2014-06-28 2016-01-27 李锦梁 Preparation method of double-salt alum

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049642A (en) * 1990-07-12 1991-03-06 江西省煤炭工业科学研究所 Stone coal ash sulfuric acid is mixed the acid slaking water logging of heating and is extracted the vanadium pentoxide technical process
CN1083023A (en) * 1992-08-25 1994-03-02 王海舟 Improved acid eduction process for producing alumina
US5895523A (en) * 1997-12-24 1999-04-20 Solv-Ex Corporation Process for making basic alkali metal sulfate pigments
CN1903727A (en) * 2005-07-26 2007-01-31 宁夏大学 Method of coproducing aluminium oxide, white carbon black and low ash carbon by coal gangue ecological utilization
JP2007106654A (en) * 2005-10-17 2007-04-26 Oji Paper Co Ltd Inorganic particle, its manufacturing method and paper using the same
CN101230419A (en) * 2007-12-29 2008-07-30 谌建开 Method for extracting vanadium pentoxide and comprehensively extracting ammonium alum and iron-oxide red from vanadium-containing stone coal or vanadium-containing ash slag

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049642A (en) * 1990-07-12 1991-03-06 江西省煤炭工业科学研究所 Stone coal ash sulfuric acid is mixed the acid slaking water logging of heating and is extracted the vanadium pentoxide technical process
CN1083023A (en) * 1992-08-25 1994-03-02 王海舟 Improved acid eduction process for producing alumina
US5895523A (en) * 1997-12-24 1999-04-20 Solv-Ex Corporation Process for making basic alkali metal sulfate pigments
CN1903727A (en) * 2005-07-26 2007-01-31 宁夏大学 Method of coproducing aluminium oxide, white carbon black and low ash carbon by coal gangue ecological utilization
JP2007106654A (en) * 2005-10-17 2007-04-26 Oji Paper Co Ltd Inorganic particle, its manufacturing method and paper using the same
CN101230419A (en) * 2007-12-29 2008-07-30 谌建开 Method for extracting vanadium pentoxide and comprehensively extracting ammonium alum and iron-oxide red from vanadium-containing stone coal or vanadium-containing ash slag

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271340A (en) * 2014-06-28 2016-01-27 李锦梁 Preparation method of double-salt alum
CN104445331A (en) * 2014-12-16 2015-03-25 兴安宸亿工贸有限公司 Method for using wastewater and waste residues generated in alum production process

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Application publication date: 20110706