CN100390061C - Method for preparing anhydrous sodium sulfite using industrial by-product anhydrous sodium sulfate - Google Patents
Method for preparing anhydrous sodium sulfite using industrial by-product anhydrous sodium sulfate Download PDFInfo
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- CN100390061C CN100390061C CNB2005100127836A CN200510012783A CN100390061C CN 100390061 C CN100390061 C CN 100390061C CN B2005100127836 A CNB2005100127836 A CN B2005100127836A CN 200510012783 A CN200510012783 A CN 200510012783A CN 100390061 C CN100390061 C CN 100390061C
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Abstract
The present invention discloses a method for preparing anhydrous sodium sulfite by using industrial by-product anhydrous sodium sulfate. In the method, sulfur dioxide furnace gas generated by burning sulfur with air is led into an acidifier to react with ash generating suspension with certain concentration in the acidifier; industrial by-product anhydrous sodium sulfate is added according to distribution ratio, calcium sulfate is precipitated and filtered to obtain sodium bisulfite, a certain amount of sodium carbonate is added stage by stage, stirring operation is slowly carried out, and sodium sulfite solution is obtained; the sodium sulfite solution is centrifugally separated to remove impurities, and sodium sulfite fine liquid can be obtained; furthermore, vacuum evaporating concentration and crystallization are carried out on the sodium sulfite fine liquid, and mother liquid is separated; vacuum drying is carried out on moisture sodium sulfite, and finished sodium sulfite can be obtained; condensed water and mother liquid are used as ash water to be recycled. The present invention effectively uses industrial by-product anhydrous sodium sulfate to realize the cyclic utilization of by-products, has no waste water, waste slag or pollution, and improves environmental protection; simultaneously, the production cost of sodium sulfite can be reduced by 30 % to 40%, funds are saved, and the economic benefit is increased by generated dihydrate gypsum.
Description
Technical field
The present invention relates to a kind of method for preparing sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate.
Background technology
At present, in processes such as Chemical Manufacture Whitfield's ointment, formic acid, tarry cut washing, all can produce the trade effluent that contains sodium sulfate, promptly pollute environment, waste resource again, strengthen the expenditure of cost and fund, unfavorable to Business survival, society is worked the mischief.
Summary of the invention
It is to overcome existing the trade effluent that contains sodium sulfate not to be handled that the present invention wants the technical solution problem, contaminate environment, the drawback of waste resource, and provide a kind of non-environmental-pollution, a kind of method for preparing sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate that economizes on resources;
The present invention prepares the method for sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate, and it can make by following step:
(1) sulphur is melted to liquid state, and insulation is to 135~140 ℃, burn at sulfur furnace with air with vaporific, controlled temperature is at 800~1000 ℃, the volume content that makes sulfurous gas in the furnace gas is 19~21%, then with furnace gas cooling, purification, the control furnace gas temperature is at 40~50 ℃, and its chemical equation is as follows:
S+O
2=SO
2
(2) make ashing suspension with S-WAT mother liquor, evaporation condensed water and unslaked lime with the certain proportion mixture slaking, its chemical equation is as follows:
CaO+H
2O=Ca(OH)
2
Ca(OH)
2+NaSO
3=CaSO
3+2NaOH
(3) the sulfurous gas furnace gas of using (1) to make again ashing suspension then carries out acidification reaction, and souring temperature is at 80~85 ℃, and acidifying terminal point pH value is 4.0~4.4;
(4) (3) acidizing fluid is put into reactor, add the industrial by-product anhydrous sodium sulphate in proportion, controlled temperature is at 80~85 ℃, stirring velocity is 10~15 rev/mins, stirs 40 minutes, after reaction is finished, left standstill in reactor two hours, and made the abundant aquation of calcium sulfate, its chemical equation is as follows:
Ca(OH)
2+SO
2=CaSO
3↓+H
2O
CaSO
3+H
2O+SO
2=Ca(HSO
3)
2
NaOH+SO
2=Na
2SO
3+H
2O
(5) with the feed liquid in (4) reactor, stir on the limit, the limit is discharged to whizzer and carries out centrifugation, gets terra alba CaSO
42H
2O, sodium bisulfite NaHSO
3Mother liquor, its chemical equation is as follows:
Ca(HSO
3)
2+Na
2SO
4+2H
2O=CaSO
4·2H
2O↓+2NaHSO
3
(6) soda ash of then the bisulfite mother liquid of sodium in (5) being put into proportional quantity neutralizes at neutralizer, control feed rate, and stirs at a slow speed, keeps temperature of reaction at 70~75 ℃, reacts two hours, and the terminal point pH value is 7.0~7.5, obtains S-WAT NaSO at last
3Solution, its chemical equation is as follows:
2NaHSO
3+Na
2CO
3=2NaSO
3+H
2O+CO
2↑
(7) again sodium sulfite solution is inserted whizzer, the centrifugation solid impurity must be made with extra care sodium sulfite solution, keeps refining sodium sulfite solution temperature at 80 ℃;
(8) the refining sodium sulfite solution of (7) gained is inserted vacuum-evaporator evaporation, crystallization, keep vacuum tightness greater than 400mmHg, vaporization temperature is controlled at more than 35 ℃, and the gained crystallization suspension contains sodium sulphite anhydrous 99.3 55~60%, the centrifugation product sodium sulphite anhydrous 99.3 NaSO that must wet
3With S-WAT NaSO
3Mother liquor;
(9) wet product sodium sulphite anhydrous 99.3 crystallization vacuum-drying, the control drying temperature is made sodium sulphite anhydrous 99.3 NaSO at last at 80~100 ℃
3Finished product.
Of the present inventionly prepare the method for sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate, its liquid-state sulfur is when sulfur furnace burns, and the weight of sulphur is 1 kilogram, and the air that drying dewaters is 380 cubic metres, the two mixed firing;
Describedly prepare the method for sodium sulphite anhydrous 99.3, contain calcium hydroxide Ca (OH) in its ashing suspension with the industrial by-product anhydrous sodium sulphate
2, calcium sulfite CaSO
3, sodium hydroxide NaOH;
Describedly prepare the method for sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate, the solid impurity that its centrifugation goes out is gone into boiler and is burned;
Describedly prepare the method for sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate, its water of condensation, S-WAT mother liquor are done the reuse of ashing water.
This method for preparing sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate provided by the present invention effectively utilizes the industrial by-product anhydrous sodium sulphate to realize the recycle of byproduct; do not produce waste water, waste residue in the whole process of production; pollution-free; strengthened environment protection; can reduce simultaneously the production cost 30~40% of S-WAT; saved fund, the dihydrate gypsum of generation also can be used as product and sells, and has increased economic benefit.
Description of drawings
Accompanying drawing is a kind of method flow synoptic diagram for preparing sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate provided by the present invention.
Embodiment
With reference to accompanying drawing, at first industrial sulphur is dropped in the sulfur melting groove 1 and be melted to liquid state, and insulation is to 135~140 ℃, install 2 after filtration with the sulphur pump then and carry out mixed firing with air through the dry back feeding of gas blower 10 moisture eliminators 11 sulfur furnace 3 with the vaporific sulfur furnace 3 of squeezing into, the weight of its sulphur is 1 kilogram, air is 380 cubic metres, controlled temperature is at 800~1000 ℃, the volume content that makes sulfurous gas in the furnace gas is 19~21%, then furnace gas is cooled off, purifies through water cooler 4, the control furnace gas temperature is at 40~50 ℃; Again 390 kilograms in S-WAT mother liquor, evaporation condensed water are squeezed into lime slaker 12 mixture slakings with unslaked lime for 3300 kilograms and make ashing suspension, contain calcium hydroxide Ca (OH) in the ashing suspension
2, calcium sulfite CaSO
3, sodium hydroxide NaOH; The materials pump is squeezed into acidifier 5 with it then, feeds the sulfurous gas furnace gas by acidifier 5 bottoms, carries out acidification reaction, and souring temperature is at 80~85 ℃, and acidifying terminal point pH value is 4.0~4.4, must contain 8% calcium bisulfite Ca (HSO
3)
2Acidizing fluid is squeezed in the reactor 6 with pump, adds 560 kilograms of industrial by-product anhydrous sodium sulphate, and controlled temperature is at 80~85 ℃, and stirring velocity is 10~15 rev/mins, stirs 40 minutes, after reaction is finished, leaves standstill in reactor 6 two hours, makes the abundant aquation of calcium sulfate; Then the stirring of the reaction solution limit in the reactor 6, limit are discharged to whizzer 13 and carry out centrifugation, get terra alba CaSO
42H
2O, sodium bisulfite NaHSO
3Mother liquor; The bisulfite mother liquid of sodium is squeezed in the neutralizer 7 with pump, kept temperature of reaction, control feed rate at 70~75 ℃, and stir at a slow speed, add soda ash in batches, reacted two hours, per hour add 210 kilograms, the terminal point pH value is 7.0~7.5, obtains S-WAT NaSO at last
3Solution; Sodium sulfite solution is inserted whizzer 14, centrifugation solid impurity, solid impurity are gone into boiler and are burned, and must make with extra care sodium sulfite solution again, keep refining sodium sulfite solution temperature at 80 ℃; The refining sodium sulfite solution of gained is inserted vacuum-evaporator 8 evaporations, crystallization, keep vacuum tightness greater than 400mmHg, vaporization temperature is controlled at more than 35 ℃, and the gained crystallization suspension contains sodium sulphite anhydrous 99.3 55~60%, the centrifugation product sodium sulphite anhydrous 99.3 NaSO that must wet
3350 kilograms and S-WAT NaSO
3380 kilograms in mother liquor; Wet product sodium sulphite anhydrous 99.3 is dry in vacuum drier 9, and the control drying temperature is made sodium sulphite anhydrous 99.3 NaSO at last at 80~100 ℃
3Finished product; Water of condensation, S-WAT mother liquor are done the reuse of ashing water.
Claims (5)
1. one kind prepares the method for sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate, it is characterized in that it can make by following step:
(1) sulphur is melted to liquid state, and insulation is burnt at sulfur furnace with air with vaporific to 135~140 ℃, controlled temperature is at 800~1000 ℃, the volume content that makes sulfurous gas in the furnace gas is 19~21%, and then with furnace gas cooling, purification, the control furnace gas temperature is at 40~50 ℃;
(2) make ashing suspension with S-WAT mother liquor, evaporation condensed water and unslaked lime with the certain proportion mixture slaking;
(3) the sulfurous gas furnace gas of using (1) to make again ashing suspension then carries out acidification reaction, and souring temperature is at 80~85 ℃, and acidifying terminal point pH value is 4.0~4.4;
(4) (3) acidizing fluid is put into reactor, add the industrial by-product anhydrous sodium sulphate in proportion, controlled temperature is at 80~85 ℃, and stirring velocity is 10~15 rev/mins, stirs 40 minutes, after reaction is finished, leaves standstill in reactor two hours, makes the abundant aquation of calcium sulfate;
(5) with the feed liquid in (4) reactor, stir on the limit, the limit is discharged to whizzer and carries out centrifugation, gets terra alba, bisulfite mother liquid of sodium;
(6) soda ash of then the bisulfite mother liquid of sodium in (5) being put into proportional quantity neutralizes at neutralizer, keeps temperature of reaction at 70~75 ℃, control feed rate, and stir at a slow speed, reacted two hours, the terminal point pH value is 7.0~7.5, obtains sodium sulfite solution at last;
(7) again sodium sulfite solution is inserted whizzer, the centrifugation solid impurity must be made with extra care sodium sulfite solution, keeps refining sodium sulfite solution temperature at 80 ℃;
(8) the refining sodium sulfite solution of (7) gained is inserted vacuum-evaporator evaporation, crystallization, keep vacuum tightness greater than 400mmHg, vaporization temperature is controlled at more than 35 ℃, and the gained crystallization suspension contains sodium sulphite anhydrous 99.3 55~60%, centrifugation must wet product sodium sulphite anhydrous 99.3 and S-WAT mother liquor;
(9) wet product sodium sulphite anhydrous 99.3 crystallization vacuum-drying, the control drying temperature is made the sodium sulphite anhydrous 99.3 finished product at last at 80~100 ℃.
2. according to the described method for preparing sodium sulphite anhydrous 99.3 with the industrial by-product anhydrous sodium sulphate of claim 1, it is characterized in that: described liquid-state sulfur is when sulfur furnace burns, the weight of its sulphur is 1 kilogram, and the air that drying dewaters is 380 cubic metres, the two mixed firing.
3. prepare the method for sodium sulphite anhydrous 99.3 according to claim 1 is described with the industrial by-product anhydrous sodium sulphate, it is characterized in that: contain calcium hydroxide, calcium sulfite, sodium hydroxide in the described ashing suspension.
4. prepare the method for sodium sulphite anhydrous 99.3 according to claim 1 is described with the industrial by-product anhydrous sodium sulphate, it is characterized in that: the solid impurity that described centrifugation goes out is gone into boiler and is burned.
5. prepare the method for sodium sulphite anhydrous 99.3 according to claim 1 is described with the industrial by-product anhydrous sodium sulphate, it is characterized in that: described water of condensation, S-WAT mother liquor are done the reuse of ashing water.
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CNB2005100127836A CN100390061C (en) | 2005-09-02 | 2005-09-02 | Method for preparing anhydrous sodium sulfite using industrial by-product anhydrous sodium sulfate |
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CNB2005100127836A CN100390061C (en) | 2005-09-02 | 2005-09-02 | Method for preparing anhydrous sodium sulfite using industrial by-product anhydrous sodium sulfate |
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CN1762809A CN1762809A (en) | 2006-04-26 |
CN100390061C true CN100390061C (en) | 2008-05-28 |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101637685B (en) * | 2009-08-24 | 2012-07-18 | 成都德美工程技术有限公司 | Comprehensive treatment method of sulfur-containing flue gas |
CN106745093B (en) * | 2016-12-17 | 2019-04-30 | 朱发彬 | Mirabilite hydrate is dehydrated the method and related molten nitre equipment of anhydrous sodium sulphate processed in a kind of chlor-alkali production |
CN106745086A (en) * | 2016-12-30 | 2017-05-31 | 耒阳市焱鑫有色金属有限公司 | One kind Ca (OH)2And SO2Multi-stage countercurrent continuously reduces Na2SO4Generation Na2SO3Reaction tower |
CN109650412B (en) * | 2018-12-28 | 2021-09-21 | 焱鑫环保科技有限公司 | Method for producing sodium sulfite by removing sulfur in sulfur-containing flue gas by arsenic-containing industrial alkaline residue |
CN109455742B (en) * | 2019-01-06 | 2021-01-12 | 曲阜师范大学 | Method for simply producing pharmaceutic adjuvant anhydrous sodium sulfite |
CN110028086A (en) * | 2019-04-12 | 2019-07-19 | 南京汇仁化工设备有限公司 | A kind of method of sulphur gas production anhydrous sodium sulfite |
CN113830794A (en) * | 2021-09-14 | 2021-12-24 | 中国神华煤制油化工有限公司 | Method and system for preparing sodium metabisulfite by utilizing sodium sulfate crystalline salt produced by coal chemical wastewater |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN87102506A (en) * | 1986-06-24 | 1988-01-06 | Fmc公司 | Improve the sodium-limestone double base of lime stone utilization rate and handle flue gas desulfurization process |
CN1165114A (en) * | 1997-02-25 | 1997-11-19 | 沈阳环境科学研究所 | Regeneration method for storage battery desulfurizing agent |
US6086842A (en) * | 1996-01-02 | 2000-07-11 | General Electric Company | Recycling of sodium hydroxide and production of gypsum from dry flue gas desulfurization |
-
2005
- 2005-09-02 CN CNB2005100127836A patent/CN100390061C/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN87102506A (en) * | 1986-06-24 | 1988-01-06 | Fmc公司 | Improve the sodium-limestone double base of lime stone utilization rate and handle flue gas desulfurization process |
US6086842A (en) * | 1996-01-02 | 2000-07-11 | General Electric Company | Recycling of sodium hydroxide and production of gypsum from dry flue gas desulfurization |
CN1165114A (en) * | 1997-02-25 | 1997-11-19 | 沈阳环境科学研究所 | Regeneration method for storage battery desulfurizing agent |
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