CN101372344A - Production method of high-purity big particle industrial anhydrous sodium sulfate - Google Patents

Production method of high-purity big particle industrial anhydrous sodium sulfate Download PDF

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Publication number
CN101372344A
CN101372344A CNA2008100310638A CN200810031063A CN101372344A CN 101372344 A CN101372344 A CN 101372344A CN A2008100310638 A CNA2008100310638 A CN A2008100310638A CN 200810031063 A CN200810031063 A CN 200810031063A CN 101372344 A CN101372344 A CN 101372344A
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anhydrous sodium
production method
imitated
heating
sodium sulfate
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CNA2008100310638A
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CN100545091C (en
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刘勇
陈伯祥
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HUNAN XINLI CHEMICAL CO Ltd
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HUNAN XINLI CHEMICAL CO Ltd
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Abstract

A method for producing high-purity large-granular industrial anhydrous sodium sulfate comprises the following steps: (1) extracting raw saltpetre water from a shaft, and injecting waste hot water into an ore bed; (2) treatment of the raw saltpetre water; (3) five-effect evaporative crystallization; (4) centrifugal dehydration; (5) drying by hot air; (6) cyclone separation; (7) sieving; and (8) quantitative packaging. The method is characterized in that the five-effect evaporative crystallization technology adopts the new production process of externally heated forced five-effect reverse circulation vacuum evaporation, which changes the normal circulation structure of the existing evaporating pot, leads the feed liquid discharged from an upper circulation tube of a heating chamber to tangentially enter a lower cone of an evaporation chamber, the feed liquid internally rotates and rises in the evaporation chamber; the clear liquid rotates along the tank center and rises to the liquid level of the evaporation chamber according to the centrifugation operating principle, and is axially discharged to a lower circulation tube after entering a central tube, then the clear liquid is cyclically reheated after entering a heating tube, the large-granular crystals downwards sediments along the evaporation chamber wall and enters a crystallizer to grow bigger. The process can enhance the average particle size of the sodium sulfate which leads the particle size being not less than 65 meshes, and can reduce dust emission, thus reducing the environment pollution.

Description

A kind of production method of high-purity big particle industrial anhydrous sodium sulfate
[technical field] the present invention relates to a kind of production method of high-purity big particle industrial anhydrous sodium sulfate, belongs to chemical technology field.
[background technology] industrial anhydrous sodium sulfate sodium suplhate is a kind of industrial chemicals that is used to wash industry, glass product, leather dyeing etc.The industrial anhydrous sodium sulphate of China as far back as last century the seventies just begin large-scale production, because production technique and the equipment that adopts was all relatively backward at that time, almost all adopt pan cooking method production anhydrous sodium sulphate, single complete equipment production capacity has only the hundreds of ton every year, industrial scale is little, poor product quality, the production cost height; At the eighties initial stage in last century, production technique improves to some extent, and Sichuan, Yuncheng, Shanxi have enterprise to begin to adopt single-action or two to imitate the natural circulation vacuum evaporation technology, throughput is increased, annual several thousand to 10,000 tons of single complete equipment production capacity, quality product increases, and cost also decreases; To the late nineteen eighties in last century, Xinjin Washing Aid Plant, Sichuan Prov., adopt and do the manufacturing of quadruple effect pump circulation vacuum evaporation technology main equipment employing stainless steel, and adopt the evaporation of cogeneration band steam turbine power generation waste heat to make the nitre technology, make single covering device production capacity reach 50,000 tons every year, quality product improves greatly, and cost further descends; Chemical plant, clear clothing river, Hongya, Sichuan after 2000, chemical plant, the Pacific Ocean, Huaian, Jiangsu are adopted V to imitate and are forced the normal circulation vacuum evaporation technology, and the chain type boiler before heat supply employing boiling type bubbling bed boiler has substituted makes single covering device production capacity annual more than 150,000 tons; Raising along with expanding economy and social consumption level, people are more and more higher to the quality of industrial anhydrous sodium sulfate product, except requiring its purity height, hardness is low, outside the whiteness height, a large number of users also needs oarse-grained industrial anhydrous sodium sulfate, the ratio that accounts for unit product as granularity 65 orders (0.234mm) of fruit product is not less than 40~50%, the flowability of product is just better, and prevented from caking, the raising of product granularity also helps reducing the grain dust pollution and surrounding enviroment are polluted, for derived product provides qualified suitable high standard raw material.This high-purity big particle industrial anhydrous sodium sulfate is still very difficult to be realized and existing production technology is produced.
[summary of the invention] the purpose of this invention is to provide a kind of production method of high-purity big particle industrial anhydrous sodium sulfate, to satisfy the demand of users to high-purity big particle industrial anhydrous sodium sulfate, improve the flowability of product, help enterprise's deep processing and reduce environmental pollution.
For solving its technical problem, the technical solution used in the present invention is: production method of the present invention comprises the steps: that 1. former glass gall is extracted in the mining area drilling well, and injects ore bed with hot water; 2. glass gall purify smart glass gall; 3. V is imitated vacuum evaporating crystalization; 4. centrifuge dehydration; 5. hot-air flow drying; 6. screening; 7. test package.
Be characterized in: it is to adopt external heating type to force V to imitate anti-circulating vacuum evaporation technology that 1. described V is imitated vacuum evaporating crystalization, this technology will have the evaporating pot normal circulation now and change anti-loop structure into, make the feed liquid of coming out from the heating chamber upper circular tube tangentially enter the lower cone of evaporator room, feed liquid spins up liter in evaporator room, the material clear liquid rises to the evaporator room liquid level position along tank body center eddy flow, enter behind the pipe core axially discharging to upper circular tube, enter the heating chamber heating that circulates once more; The big crystal of particle enters crystallizer and continues to grow up along the downward sedimentation of evaporation tank skin, becomes the big and product uniformly of granularity at last.
2. described external heating type forces V to imitate anti-circulating vacuum evaporation technology, be that the low pressure saturated vapo(u)r that the steam that adopts raw coal to produce by circulating fluidized bed boiler promotes after the turbo-generator generating is a back pressure steam, flow to the evaporating pot heating, end effect secondary steam after the heating is through the follow-up continuous hot tub cooling that circulates once more that is transported to of recirculated water condensation step by step, other various waste water flow into the used heat pond, through waterflood pump, the spent hot water is injected in the mine again.
3. the processing parameter that described V is imitated anti-circulating vacuum evaporation is: it is gauge pressure 0.293Mpa that I is imitated heated pressure, 128 ℃ of feed temperatures, and it is gauge pressure-0.097Mpa that V is imitated evaporator room pressure, 43.5 ℃ of feed temperatures, each imitates heat transfer area 1100m 2
What the forced circulation pump of heating pump circulation vacuum evaporation technology adopted outside 4. described V was imitated is the HZ-1000 propeller pump.
What 5. described glass gall was handled employing is chemistry and physical method deliming, demagging, iron removal technology.
The present invention compared with prior art has following beneficial effect:
1. because the present invention adopts crossover circulation technique, improved the mean particle size of sodium sulfate crystal greatly, granular level reaches D 50〉=65 orders, owing to adopt HZ-1000 pump circulation propeller pump, make flow reach 12000 cubic meters/hours, add advanced glass gall treatment process, reduce the hardness of product widely, eliminated impurity, increased the whiteness of product, thereby the quality and the performance of product have been improved, according to detecting the standard that its quality product meets or exceeds national GB GB/T6009-2003I class acceptable end product fully.
2. because the present invention adopts V to imitate anti-circulating vacuum evaporation new process of production, the dust content in the production process is significantly reduced,, improve Working environment and created good condition for reducing dust pollution.
3. the product of producing with production method of the present invention is compared with GB GB/T6009-2003, and every index all is higher than GB, and concrete contrast table is as described below:
Index name GB worker's class acceptable end product The product that the present invention produces
The sulfuric acid steel is (with Na 2SO 4Count) content % 〉= 99.0 99.1
The insoluble content % of water≤ 0.05 0.02
Calcium, magnesium (in mg) total content %≤ 0.15 0.02
Muriate (in cl) content %≤ 0.35 0.30
Iron (in fe) content %≤ 0.002 0.0006
Moisture content≤ 0.20 0.03
Whiteness 〉= 82 88
Granularity D 50mm 65 orders
[embodiment] mask body down introduces the production method of producing 600000 tons of high-purity big particle industrial anhydrous sodium sulfates in 1 year per year.This production method comprises the steps: 1. to extract with HZ-1000 pump circulation propeller pump the former glass gall of contains sodium sulfate from mine; 2. glass gall is handled: former glass gall in reaction container, by physics and chemical reaction, is obtained smart glass gall after removing de-iron, magnesium, calcium impurities; 3. V is imitated (containing multiple-effect) evaporative crystallization: adopt external heating type to force V to imitate anti-circulating vacuum evaporation technology, this technology is with existing evaporating pot normal circulation structure, change anti-loop structure into, making the feed liquid of coming out from the heating chamber upper circular tube is described smart glass gall, tangentially enter the lower cone of evaporator room, feed liquid spins up liter in evaporator room, the body that particle is little enters down circulation tube with clear liquid after tank body center eddy flow rises to pipe core, enter the heating chamber heating that circulates once more, the big crystal of particle is along the downward sedimentation of evaporation tank skin, enter crystallizer and continue to grow up, obtain granularity product greatly and uniformly.Wherein add thermal recovery raw coal and the circulating fluidized bed boiler of evaporating pot produce steam, the heating chamber of delivering to evaporating pot with the low pressure saturated vapo(u)r after the steam drive generator for electricity generation heats smart glass gall, V effect secondary steam becomes hot water and enters hot tub after the recirculated water cooling, this hot water is after water pump is delivered to the cooling tower cooling, low-temperature receiver as cooling V effect secondary steam recycles once more, various factory effluents are sent into wastewater disposal basin, send mine back to waterflood pump, wherein, the temperature that I is imitated heating chamber is 143 ℃, and the pressure of heating chamber is gauge pressure 0.293Mpa; It is gauge pressure-0.093Mpa that V is imitated evaporator room pressure, and evaporator room liquid temperature is 43.5 ℃, and the secondary steam temperature is 41 ℃, and each imitates heat transfer area 1100m 24. centrifuge dehydration: the slurry of the nitre after the evaporation concentration is put into nitre slurry bucket, use centrifuge dewatering then, obtain water content≤3% sodium sulfate; 5. warm air drying: adopt hot blast to carry out drying to wet sodium sulfate and obtain solid sodium sulfate; 6. cyclonic separation: dried solid sodium sulfate separated obtaining the exsiccant anhydrous sodium sulphate with hot blast; 7. screening: multilayer is revolved the sieve teacher branch that shakes and is obtained qualified anhydrous sodium sulphate product; 8. weighing is the high-purity big particle industrial anhydrous sodium sulfate finished product behind the test package.

Claims (5)

1. the production method of a high-purity big particle industrial anhydrous sodium sulfate comprises the steps: that 1. mining area drilling well extracts former glass gall and inject ore bed with the spent hot water; 2. former glass gall is purified, obtain smart glass gall; 3. V is imitated vacuum evaporating crystalization; 4. centrifuge dehydration; 5. warm air drying; 6. screening; 7. check, packing, it is characterized in that: it is to adopt external heating type to force V to imitate anti-circulating vacuum evaporation technology that described V is imitated vacuum evaporating crystalization, this technology will have the evaporating pot normal circulation now and change anti-loop structure into, make the feed liquid of coming out from the heating chamber upper circular tube tangentially enter the lower cone of evaporator room, feed liquid spins up liter in evaporator room, and the material clear liquid rises to the evaporator room liquid level position along tank body center eddy flow, enter behind the pipe core axially discharging to upper circular tube, enter the heating chamber heating that circulates once more; The big crystal of particle enters crystallizer and continues to grow up along the downward sedimentation of evaporation tank skin, becomes the big and product uniformly of granularity at last.
2. according to the production method of the described anhydrous sodium sulphate of claim 1, it is characterized in that: described external heating type forces V to imitate anti-circulating vacuum evaporation technology, be that the low pressure saturated vapo(u)r that the steam that adopts raw coal to produce by circulating fluidized bed boiler promotes after the turbo-generator generating is a back pressure steam, flow to the evaporating pot heating, end effect secondary steam after the heating is through the follow-up continuous hot tub cooling that circulates once more that is transported to of recirculated water condensation step by step, other various waste water flow into the used heat pond, through waterflood pump, the spent hot water is injected in the mine again.
3. according to the production method of the described anhydrous sodium sulphate of claim 1, it is characterized in that: the processing parameter that described V is imitated anti-circulating vacuum evaporation is: it is gauge pressure 0.293Mpa that I is imitated heated pressure, 128 ℃ of feed temperatures, it is gauge pressure-0.097Mpa that V is imitated evaporator room pressure, 43.5 ℃ of feed temperatures, each imitates heat transfer area 1100m 2
4. according to the production method of the described anhydrous sodium sulphate of claim 1, it is characterized in that: what the forced circulation pump of heating pump circulation vacuum evaporation technology adopted outside described V was imitated is the HZ-1000 propeller pump.
5. according to the production method of the described anhydrous sodium sulphate of claim 1, it is characterized in that: what described glass gall was handled employing is chemistry and physical method deliming, demagging, iron removal technology.
CNB2008100310638A 2008-04-10 2008-04-10 A kind of production method of high-purity big particle industrial anhydrous sodium sulfate Expired - Fee Related CN100545091C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101928020A (en) * 2010-05-21 2010-12-29 四川省川眉芒硝有限责任公司 Continuous crystallization manufacturing process of medicinal glauber salt
CN102180487A (en) * 2011-03-30 2011-09-14 湖南新澧化工有限公司 Method for recycling saltpeter-production dead steam
WO2011140855A1 (en) * 2010-05-10 2011-11-17 Xu Daren Process for directly obtaining anhydrous sodium sulfate by flash evaporating and crystallizing and apparatus thereof
CN101837994B (en) * 2009-03-20 2012-01-11 四川省川眉芒硝有限责任公司 Production process of medicinal mirabilite
CN103086403A (en) * 2013-02-06 2013-05-08 四川省洪雅青衣江元明粉有限公司 Anhydrous sodium sulfate preparation method and anhydrous sodium sulfate preparation apparatus
CN109592698A (en) * 2018-12-12 2019-04-09 天津大学 A method of preparing funnel-form sodium sulphate from high-salt wastewater

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837994B (en) * 2009-03-20 2012-01-11 四川省川眉芒硝有限责任公司 Production process of medicinal mirabilite
WO2011140855A1 (en) * 2010-05-10 2011-11-17 Xu Daren Process for directly obtaining anhydrous sodium sulfate by flash evaporating and crystallizing and apparatus thereof
CN101928020A (en) * 2010-05-21 2010-12-29 四川省川眉芒硝有限责任公司 Continuous crystallization manufacturing process of medicinal glauber salt
CN101928020B (en) * 2010-05-21 2011-11-23 四川省川眉芒硝有限责任公司 Continuous crystallization manufacturing process of medicinal glauber salt
CN102180487A (en) * 2011-03-30 2011-09-14 湖南新澧化工有限公司 Method for recycling saltpeter-production dead steam
CN103086403A (en) * 2013-02-06 2013-05-08 四川省洪雅青衣江元明粉有限公司 Anhydrous sodium sulfate preparation method and anhydrous sodium sulfate preparation apparatus
CN109592698A (en) * 2018-12-12 2019-04-09 天津大学 A method of preparing funnel-form sodium sulphate from high-salt wastewater

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