CN102674412A - Preparation method of magnesium chloride hexahydrate - Google Patents
Preparation method of magnesium chloride hexahydrate Download PDFInfo
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- CN102674412A CN102674412A CN201210203729XA CN201210203729A CN102674412A CN 102674412 A CN102674412 A CN 102674412A CN 201210203729X A CN201210203729X A CN 201210203729XA CN 201210203729 A CN201210203729 A CN 201210203729A CN 102674412 A CN102674412 A CN 102674412A
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Abstract
The invention discloses a preparation method of magnesium chloride hexahydrate, which comprises the steps of: preheating the mother liquor for bromide preparation which has the magnesium chloride content of 360g/l-470g/l and the specific gravity of 32-37.5 degrees Be'; after the temperature reaches 80-90 DEG C, sending the mother liquor for bromide preparation into an evaporation tank for evaporating under the conditions that the vapor pressure is 0.35-0.6MPa and the vacuum degree is -0.067 to -0.085 MPa; and after the material liquid reaches the termination boiling point temperature of 121-136 DEG C, carrying out heat preservation and sedimentation, cooling, flaking, metering and packaging. Since the vacuum degree in the evaporation tank is improved, the termination boiling point temperature of the material liquid is reduced, the evaporation time is shortened, the evaporation energy consumption is lowered and the tank cleaning cycle is prolonged, and the production efficiency is improved further.
Description
Technical field
The present invention relates to the preparation method of magnesium chloride hexahydrate, being specially a kind of is the preparation method of the magnesium chloride hexahydrate of raw material with system bromine mother liquor.
Background technology
At present, the raw material of producing magnesium chloride hexahydrate is generally with the mother liquor behind the system bromine, and system bromine mother liquor is a kind of undersaturated magnesium chloride brine, needs evaporation concentration, just can produce the magnesium chloride hexahydrate product.Usually take two kinds of methods of atmospheric evaporation and reduction vaporization.Atmospheric evaporation is system bromine mother liquor to be put into open container under atmospheric pressure carry out heating evaporation and concentrate; Decompression (vacuum) evaporation is that bromine extraction waste brine is put into Sealing Arrangement, is being lower than under the normal atmosphere (vacuum tightness-below the 0.066Mpa) heating evaporation, secondary steam is introduced condensation obtains certain vacuum in the mixing condenser.
The magnesium chloride brine boiling point is high, and facile hydrolysis is fit to reduction vaporization.Though adopt normal pressure still reduction vaporization concentrate and make the bromine mother liquor, all be under boiling state with water vapor, magnesium chloride solution concentration is constantly increased.When content of magnesium chloride enrichment in the feed liquid arrives the production technique standard-required, promptly stop evaporation.
The problem that tradition magnesium chloride hexahydrate production technique exists is: evaporation requires the termination boiling point temperature high, and more than 136 ℃, evaporation time is longer, and generally more than 90 minutes, steam consumption makes that more than 25 tons the brush jar cycle is short, is about 3 days.
Summary of the invention
For solving the problem that exists in the above-mentioned production technique, the present invention provides a kind of preparation method of magnesium chloride hexahydrate, may further comprise the steps:
1. preheating: with content of magnesium chloride is 360g/l-470 g/l, and proportion is that the system bromine mother liquor of 32-37.5 ° of Be ' is sent into preheater, is heated to 80-90 ℃;
2. vacuum-evaporation: the system bromine mother liquor after the preheating sent in the evaporating pot evaporate, wherein, the vapor pressure of heating chamber is 0.35Mpa-0.6Mpa, and the vacuum tightness of evaporator room is-and 0.067Mpa is to-0.085Mpa;
3. be incubated sedimentation: the feed liquid after the vacuum-evaporation is reached discharge insulation sedimentation after 121-136 ℃ of the termination boiling point temperature;
4. cool off film-making: will be incubated feed liquid after the sedimentation through pelleter cooling film-making, product thickness is 2-4mm;
5. pack: the finished product magnesium chloride hexahydrate of 2-4mm is pulverized transmission through worm conveyor, to packing the hopper packing.
Evaporating pot used in the present invention comprises heating chamber and evaporator room, and wherein, heating chamber adopts shell and tube heat exchanger, and feed liquid is in the tubulation internal flow, and steam is in the tubulation Clearance Flow, and steam gives tubulation inner feed liquid heating through heat passage.
Technical scheme of the present invention brings up to the vacuum tightness of evaporator room-and 0.067Mpa is to-0.085Mpa, and then feed liquid termination boiling point temperature drops to 121-136 ℃, and evaporation time foreshortens to 65-85 minute; Steam consumption is reduced to the 18-23 ton; Brush jar cycle stretch-out was to 7-10 days, and energy consumption reduces, and production efficiency improves.
Description of drawings
Fig. 1 prepares the magnesium chloride hexahydrate technological process block-diagram for system bromine mother liquor.
Embodiment
The vacuum tightness corresponding relation such as the following table of evaporation termination boiling point temperature and evaporator room
Can find out that through last table vacuum tightness is high more, the termination boiling point temperature is low more.If the termination boiling point temperature is higher, magnesium chloride solution is prone to hydrolytic reactions, etching apparatus; If the termination boiling point temperature is during than sinking to the 116 degree left and right sides, feed liquid will be condensed, and evaporation operation can't be carried out.
This technology is the result who under the prerequisite of above two kinds of influence factors, takes all factors into consideration, and below is the specific embodiment of technical scheme of the present invention:
Embodiment 1:
Content of magnesium chloride is 360g/l in the system bromine mother liquor, and proportion is 33.5 ° of Be ', and the temperature of system bromine mother liquor is 80 ℃ after the preheating, and vapor pressure is 0.35 Mpa in the evaporating pot heating chamber, and vacuum tightness is-0.067Mpa in the evaporator room.Vouch that through producing complete evaporation of liquid termination boiling point temperature is 136 ℃, one jar of feed liquid evaporation time is 99 minutes, and steam economy is 22.56t, and the content of magnesium chloride is 46.5% (quality percentage composition) in the complete evaporation of liquid.
Embodiment 2:
Content of magnesium chloride is 360g/l in the system bromine mother liquor, and proportion is 33.5 ° of Be ', and the temperature of system bromine mother liquor is 90 ℃ after the preheating, and vapor pressure is 0.6 Mpa in the evaporating pot heating chamber, and vacuum tightness is-0.085Mpa in the evaporator room.Vouch that through producing complete evaporation of liquid termination boiling point temperature is 121 ℃, one jar of feed liquid evaporation time is 75 minutes, and steam economy is 19t, and the content of magnesium chloride is 46.7% in the complete evaporation of liquid.
Embodiment 3:
Content of magnesium chloride is 410g/l in the system bromine mother liquor, and proportion is 35.0 ° of Be ', and the temperature of system bromine mother liquor is 90 ℃ after the preheating, and vapor pressure is 0.45 Mpa in the evaporating pot heating chamber, and vacuum tightness is-0.075Mpa in the evaporator room.Vouch that through producing complete evaporation of liquid termination boiling point temperature is 130 ℃, one jar of feed liquid evaporation time is 79 minutes, and steam economy is 19.3t, and the content of magnesium chloride is 47.0% in the complete evaporation of liquid.
Embodiment 4:
Content of magnesium chloride is 470g/l in the system bromine mother liquor, and proportion is 37.5 ° of Be ', and the temperature of system bromine mother liquor is 90 ℃ after the preheating, and vapor pressure is 0.6 Mpa in the evaporating pot heating chamber, and vacuum tightness is-0.080Mpa in the evaporator room.Vouch that through producing complete evaporation of liquid termination boiling point temperature is 125 ℃, one jar of feed liquid evaporation time is 73 minutes, and steam economy is 16.32t, and the content of magnesium chloride is 47.1% in the complete evaporation of liquid.
Embodiment 5:
Content of magnesium chloride is 470g/l in the system bromine mother liquor, and proportion is 37.5 ° of Be ', and the temperature of system bromine mother liquor is 90 ℃ after the preheating, and vapor pressure is 0.6 Mpa in the evaporating pot heating chamber, and vacuum tightness is-0.085Mpa in the evaporator room.Vouch that through producing complete evaporation of liquid termination boiling point temperature is 121 ℃, one jar of feed liquid evaporation time is 69 minutes, and steam economy is 16t, and the content of magnesium chloride is 47.2% in the complete evaporation of liquid.
The present invention passes through moderately gas clean-up, has shortened evaporation time, has practiced thrift steam consumption, has improved production efficiency.
Claims (1)
1. the preparation method of a magnesium chloride hexahydrate may further comprise the steps:
1. preheating: with content of magnesium chloride is 360g/l-470 g/l, and proportion is that the system bromine mother liquor of 32-37.5 ° of Be ' is sent into preheater, is heated to 80-90 ℃;
2. vacuum-evaporation: the system bromine mother liquor after the preheating sent in the evaporating pot evaporate, wherein, the vapor pressure of heating chamber is 0.35Mpa-0.6Mpa, and the vacuum tightness of evaporator room is-and 0.067Mpa is to-0.085Mpa;
3. be incubated sedimentation: the feed liquid after the vacuum-evaporation is reached discharge insulation sedimentation after 121-136 ℃ of the termination boiling point temperature;
4. cool off film-making: will be incubated feed liquid after the sedimentation through pelleter cooling film-making, product thickness is 2-4mm;
5. pack: the finished product magnesium chloride hexahydrate of 2-4mm is pulverized transmission through worm conveyor, to packing the hopper packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210203729XA CN102674412A (en) | 2012-06-20 | 2012-06-20 | Preparation method of magnesium chloride hexahydrate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210203729XA CN102674412A (en) | 2012-06-20 | 2012-06-20 | Preparation method of magnesium chloride hexahydrate |
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| CN102674412A true CN102674412A (en) | 2012-09-19 |
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| CN201210203729XA Pending CN102674412A (en) | 2012-06-20 | 2012-06-20 | Preparation method of magnesium chloride hexahydrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145159A (en) * | 2013-03-26 | 2013-06-12 | 连云港日丰钙镁有限公司 | Production process of magnesium chloride granules |
| CN104274994A (en) * | 2013-07-01 | 2015-01-14 | 天津长芦汉沽盐场有限责任公司 | Continuous crystallization production method for crystal magnesium chloride |
| CN106006686A (en) * | 2016-08-16 | 2016-10-12 | 天津海光药业股份有限公司 | Technology for producing magnesium chloride with medicinal application |
| CN107879364A (en) * | 2017-12-04 | 2018-04-06 | 大连盐化集团有限公司 | A kind of preparation method of food-grade magnesium chloride hexahydrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1099008A (en) * | 1993-08-19 | 1995-02-22 | 天津长芦塘沽盐场 | Bittern prepares the new process of production of white magnesium chloride |
| CN1429769A (en) * | 2001-12-30 | 2003-07-16 | 山东海化集团有限公司 | Method of preparing white magnesium chloride by reduction method |
| US20040009869A1 (en) * | 2002-07-15 | 2004-01-15 | Wagner Burkhard Eric | Enhanced solubility of magnesium halides and catalysts and polymerization process using same |
-
2012
- 2012-06-20 CN CN201210203729XA patent/CN102674412A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1099008A (en) * | 1993-08-19 | 1995-02-22 | 天津长芦塘沽盐场 | Bittern prepares the new process of production of white magnesium chloride |
| CN1429769A (en) * | 2001-12-30 | 2003-07-16 | 山东海化集团有限公司 | Method of preparing white magnesium chloride by reduction method |
| US20040009869A1 (en) * | 2002-07-15 | 2004-01-15 | Wagner Burkhard Eric | Enhanced solubility of magnesium halides and catalysts and polymerization process using same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145159A (en) * | 2013-03-26 | 2013-06-12 | 连云港日丰钙镁有限公司 | Production process of magnesium chloride granules |
| CN104274994A (en) * | 2013-07-01 | 2015-01-14 | 天津长芦汉沽盐场有限责任公司 | Continuous crystallization production method for crystal magnesium chloride |
| CN106006686A (en) * | 2016-08-16 | 2016-10-12 | 天津海光药业股份有限公司 | Technology for producing magnesium chloride with medicinal application |
| CN107879364A (en) * | 2017-12-04 | 2018-04-06 | 大连盐化集团有限公司 | A kind of preparation method of food-grade magnesium chloride hexahydrate |
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Application publication date: 20120919 |