CN1128105C - Sodium carbonate extracting process from caustic lime containing sodium sulfate - Google Patents
Sodium carbonate extracting process from caustic lime containing sodium sulfate Download PDFInfo
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- CN1128105C CN1128105C CN 00113582 CN00113582A CN1128105C CN 1128105 C CN1128105 C CN 1128105C CN 00113582 CN00113582 CN 00113582 CN 00113582 A CN00113582 A CN 00113582A CN 1128105 C CN1128105 C CN 1128105C
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- Prior art keywords
- sodium carbonate
- crystal
- sodium
- liquor
- soda ash
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 title claims abstract description 86
- 229910000029 sodium carbonate Inorganic materials 0.000 title claims abstract description 43
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 18
- 229910052938 sodium sulfate Inorganic materials 0.000 title claims abstract description 18
- 235000011152 sodium sulphate Nutrition 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 title 1
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 42
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 34
- 239000013078 crystal Substances 0.000 claims abstract description 29
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 17
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 17
- 229940001593 sodium carbonate Drugs 0.000 claims abstract description 17
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 11
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 9
- XYQRXRFVKUPBQN-UHFFFAOYSA-L Sodium carbonate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]C([O-])=O XYQRXRFVKUPBQN-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229940018038 sodium carbonate decahydrate Drugs 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000003463 adsorbent Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 abstract 3
- 229940076133 sodium carbonate monohydrate Drugs 0.000 abstract 3
- 239000003610 charcoal Substances 0.000 abstract 2
- 239000000843 powder Substances 0.000 abstract 2
- 239000002002 slurry Substances 0.000 abstract 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 238000007127 saponification reaction Methods 0.000 description 5
- 239000000284 extract Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- -1 organic acid sodium-salt Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Fertilizers (AREA)
- Processing Of Solid Wastes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for extracting sodium carbonate from soda ash containing sodium sulfate, which is characterized in that soda ash and desalted water are continuously stirred and dissolved to adsorb impurities in the solution by utilizing charcoal powder, and then, the solution is filtered to obtain the charcoal powder and filter liquor A which is evaporated and crystallized to obtain crystal slurry liquor containing a sodium carbonate monohydrate crystal which is filtered to obtain the sodium carbonate monohydrate crystal and filter liquor B; ammonium bicarbonate is added into the filter liquor B to react with the sodium sulfate to generate sodium bicarbonate and ammonium sulfate. The mixed liquor after the reaction is cooled and crystallized, and the crystal slurry liquor formed by crystallization is filtered to obtain a sodium carbonate decahydrate crystal, a sodium bicarbonate crystal and filter liquor C. The sodium carbonate decahydrate crystal, the sodium bicarbonate crystal and the sodium carbonate monohydrate crystal are calcined together to obtain the heavy sodium carbonate with a high content.
Description
The present invention relates to a kind of method of from the sode ash that contains sodium sulfate, extracting yellow soda ash, be particularly suitable for from the sode ash that contains a small amount of sodium sulfate that saponification waste lye burning back produces, extracting yellow soda ash.
Saponification liquor is to produce in some Chemicals process with the waste liquid that produces with organic acid in the alkali, contain organic acid sodium-salt, it produces a kind of pulverous sode ash through the burning back, the fuel used heavy oil that is generally, contain a small amount of sulphur in the heavy oil, sulphur is sodium sulfate with saponification liquor incendiary product, it and organic acid sodium salt products of incomplete combustion carbon dust are mixed in the sode ash, reduced the sode ash quality, and increased refining difficulty, can only sell glasswork with the price below 500 yuan per ton and make raw material, economic benefit is low.The tap density of sode ash and granularity are all less in addition, easily produce dust in transportation and the use, and loss is big, and environment and HUMAN HEALTH are also had certain influence.
The object of the present invention is to provide a kind of method of from the sode ash that contains a small amount of sodium sulfate that saponification waste lye burning back produces, making with extra care extraction yellow soda ash.Comprise steps such as dissolving and absorption, filtration, evaporative crystallization, filtration, drying, reaction, crystallisation by cooling, filtration.
The present invention is achieved in that
A. with sode ash and de-salted water with 1: 2～4 weight ratio mix the back continuously stirring make sode ash dissolve alkaline solution, utilize the impurity in the carbon dust absorption sode ash in the sode ash simultaneously, dissolving and adsorption temp are 30～100 ℃, are preferably 60～70 ℃, then
B. alkaline solution is filtered to get filtrate A and carbon dust, then
C. with filtrate A evaporative crystallization, the form that makes yellow soda ash be monohydrated sodium carbonate is separated out, and vaporization temperature is 50～100 ℃, being preferably 60～70 ℃, evaporating pressure is-0.02～-0.1Mpa, be preferably-0.06～0.1Mpa, steam output is 20～60wt% of filtrate total amount, is preferably 30～40wt%, then
D. will evaporate the back gained magma liquid filter monohydrated sodium carbonate crystal and liquor B, then
E. the monohydrated sodium carbonate crystal is calcined heavy yellow soda ash.Calcining temperature is 120～270 ℃, then
F. add bicarbonate of ammonia and sodium sulfate reaction generation sodium bicarbonate and ammonium sulfate in liquor B, temperature of reaction is 30～80 ℃, and the weight ratio of sodium sulfate is 1.0～2.0: 1 in the bicarbonate of ammonia of adding and the liquor B, is preferably 1.6～1.7: 1, then
G. with reacted mixed solution crystallisation by cooling, ammonium sulfate is bigger because of solubleness, still is dissolved in the solution, and sodium bicarbonate and yellow soda ash are crystal state together and separate out.The crystallisation by cooling temperature is 5～30 ℃, is preferably 10～20 ℃, then
H. the magma liquid that crystallisation by cooling is formed filter the crystal and the liquor C of Sodium carbonate decahydrate and sodium bicarbonate, then
I. yellow soda ash and sodium bicarbonate crystal with the monohydrated sodium carbonate crystal of steps d gained calcine heavy yellow soda ash.Liquor C is the ammoniumsulphate soln that contains a small amount of yellow soda ash, can be made into ammonium sulfate fertilizer.
Fig. 1 is the refining technological process block-diagram that extracts yellow soda ash of sode ash.
Extract high-quality heavy the sode ash that good effect of the present invention is to produce after the saponification liquor burning Matter sodium carbonate has higher economic benefit, produces 5000 tons of sode ashs per year through the refining carbon that extracts of said method Can create about 2,000,000 yuan of effects behind the acid sodium, and be conducive to environmental protection, avoid the lightweight sode ash in a large number floating Phenomenon.
Embodiment 1. gets 1500g sode ash and 3750g de-salted water 70 ℃ of following continuously stirring dissolvings, and utilizes the impurity in the carbon dust adsorbent solution under this temperature, filter then carbon dust and filtrate A.Filtrate A 70 ℃ and-0.093Mpa under evaporative crystallization obtain containing monohydrated sodium carbonate crystalline magma liquid, steam output is 50wt%, magma liquid filter monohydrated sodium carbonate crystal and liquor B, add bicarbonate of ammonia and sodium sulfate and react generation sodium bicarbonate and ammonium sulfate down at 70 ℃ in liquor B, the weight ratio of sodium sulfate is 1.6: 1 in the bicarbonate of ammonia of adding and the liquor B.At 15 ℃ of following crystallisation by cooling, ammonium sulfate is carried on as before and so is dissolved in the solution with reacted mixed solution, and sodium bicarbonate and yellow soda ash are crystal state together and separate out.The magma liquid that crystallisation by cooling is formed filter the crystal and the liquor C of Sodium carbonate decahydrate and sodium bicarbonate.Yellow soda ash and sodium bicarbonate crystal with the monohydrated sodium carbonate crystal of front gained calcine heavy yellow soda ash, carbonate content is 99.45wt%.
Embodiment 2. gets 1500g sode ash and 3750g de-salted water 60 ℃ of following continuously stirring dissolvings, and utilizes the impurity in the carbon dust adsorbent solution under this temperature, filter then carbon dust and filtrate A.Filtrate A 60 ℃ and-0.093Mpa under evaporative crystallization obtain containing monohydrated sodium carbonate crystalline magma liquid, steam output is 30wt%, magma liquid filter monohydrated sodium carbonate crystal and liquor B, add bicarbonate of ammonia and sodium sulfate and react generation sodium bicarbonate and ammonium sulfate down at 60 ℃ in liquor B, the weight ratio of sodium sulfate is 1.7: 1 in the bicarbonate of ammonia of adding and the liquor B.At 20 ℃ of following crystallisation by cooling, ammonium sulfate is carried on as before and so is dissolved in the solution with reacted mixed solution, and sodium bicarbonate and yellow soda ash are crystal state together and separate out.The magma liquid that crystallisation by cooling is formed filter the crystal and the liquor C of Sodium carbonate decahydrate and sodium bicarbonate.Yellow soda ash and sodium bicarbonate crystal with the monohydrated sodium carbonate crystal of front gained calcine heavy yellow soda ash, carbonate content is 99.58wt%.
Claims (2)
1. method of extracting yellow soda ash from the sode ash that contains sodium sulfate is characterized in that being made of following steps:
A. with sode ash and de-salted water with 1: 2～4 weight ratio mix the back continuously stirring make sode ash dissolve alkaline solution, utilize contained impurity in the carbon dust adsorbent solution in the sode ash simultaneously, dissolving and adsorption temp are 30～100 ℃, then
B. alkaline solution is filtered to get filtrate A and carbon dust, then
C. with filtrate A evaporative crystallization, the form that makes yellow soda ash be monohydrated sodium carbonate is separated out, and vaporization temperature is 50～100 ℃, and evaporating pressure is-0.02～-0.1MPa, steam output is 20～60wt% of filtrate total amount, then
D. will evaporate the back gained magma liquid filter monohydrated sodium carbonate crystal and liquor B, then
E. the monohydrated sodium carbonate crystal is calcined heavy yellow soda ash, calcining temperature is 120～270 ℃, then
F. add bicarbonate of ammonia and sodium sulfate reaction generation sodium bicarbonate and ammonium sulfate in liquor B, temperature of reaction is 30～80 ℃, and the weight ratio of sodium sulfate is 1.0～2.0: 1 in the bicarbonate of ammonia of adding and the liquor B, then
G. with reacted mixed solution crystallisation by cooling, ammonium sulfate is bigger because of solubleness, still is dissolved in the solution, and sodium bicarbonate and yellow soda ash are crystal state together separates out, and the crystallisation by cooling temperature is 5～30 ℃, then
H. the magma liquid that crystallisation by cooling is formed filter the crystal and the liquor C of Sodium carbonate decahydrate and sodium bicarbonate, then
I. Sodium carbonate decahydrate and sodium bicarbonate monohydrated sodium carbonate in steps d calcine heavy yellow soda ash.
2. a kind of method of from the sode ash that contains sodium sulfate, extracting yellow soda ash according to claim 1, it is characterized in that: dissolving, the adsorption temp in a step are 60～70 ℃, the vaporization temperature in c step is 60～70 ℃, evaporating pressure is-0.06～-0.1MPa, steam output is 30～40wt%, the weight ratio in f step is 1.6～1.7: 1, and the crystallisation by cooling temperature in g step is 10～20 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00113582 CN1128105C (en) | 2000-07-29 | 2000-07-29 | Sodium carbonate extracting process from caustic lime containing sodium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00113582 CN1128105C (en) | 2000-07-29 | 2000-07-29 | Sodium carbonate extracting process from caustic lime containing sodium sulfate |
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| CN1336324A CN1336324A (en) | 2002-02-20 |
| CN1128105C true CN1128105C (en) | 2003-11-19 |
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| CN 00113582 Expired - Fee Related CN1128105C (en) | 2000-07-29 | 2000-07-29 | Sodium carbonate extracting process from caustic lime containing sodium sulfate |
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| CN110980743A (en) * | 2019-12-26 | 2020-04-10 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | Method for preparing sodium fluoride and white carbon black by using caprolactam waste alkali |
| CN113998712A (en) * | 2021-11-18 | 2022-02-01 | 江苏力波兴水务科技有限公司 | A kind of method for removing chloride ion from alkali ash filtrate and recovering sodium sulfate and sodium carbonate |
| CN114538477B (en) * | 2022-04-27 | 2022-09-02 | 天津渤化永利化工股份有限公司 | Improved production method of heavy soda ash |
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| CN1336324A (en) | 2002-02-20 |
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Granted publication date: 20031119 Termination date: 20190729 |