CN102320633B - Method for producing basic magnesium carbonate by boron sludge - Google Patents
Method for producing basic magnesium carbonate by boron sludge Download PDFInfo
- Publication number
- CN102320633B CN102320633B CN2011102531586A CN201110253158A CN102320633B CN 102320633 B CN102320633 B CN 102320633B CN 2011102531586 A CN2011102531586 A CN 2011102531586A CN 201110253158 A CN201110253158 A CN 201110253158A CN 102320633 B CN102320633 B CN 102320633B
- Authority
- CN
- China
- Prior art keywords
- jar
- slip
- temperature
- carbonization
- squeezed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Processing Of Solid Wastes (AREA)
- Fertilizers (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention is a method for producing basic magnesium carbonate by boron sludge. The invention comprises the process steps of boron sludge drying processing, material preparation, size mixing, carbonization, finished product preparation, etc. Compared with the prior art, the invention does not require boron sludge roasting; boric acid mother liquor discharged from boron magnesium ore processing by a hydrochloric acid method is used for material preparation; a size mixing procedure is added; the heating temperature is changed; water is saved; the labor intensity of production workers is low; the operation is convenient; the energy consumption is low; the carbonization time is short. The invention can realize ten-thousand DWT large-scale production and re-expanded production. After basic magnesium carbonate extraction from boron sludge, the magnesium sludge can be used to produce microelement fertilizer and non-burnt bricks necessary for ecological agriculture, which realizes the comprehensive utilization of resources.
Description
Technical field
The present invention relates to a kind of Chemicals preparation method, promptly utilize boron mud to produce the method for magnesium basic carbonate.
Background technology
In the prior art, the waste residue boron mud that produces during borax is produced generally contains the Natural manganese dioxide more than 30% in boron mud.Boron mud often is used as waste material and abandons, contaminate environment.
People are pursuing the utilization of waste material of boron mud always.Report to the utilization of boron mud mainly was to be used for producing magnesium basic carbonate in recent years.Magnesium basic carbonate is a kind of important chemical material, is mainly used in ceramic industry, opticglass, daily-use chemical industry and rubber industry, and common price is at 3500～4000 yuan/ton on the market.Boron mud is the important source material of producing the high-quality magnesium basic carbonate.With boron mud is that raw material is produced the shortcoming that magnesium basic carbonate exists and is: the one, be crushed to brick to boron mud through brick press earlier, and pass through brickkiln or shaft furnace roasting again.It is of poor quality and unstable to burn the boron adobe that, and power consumption is high, severe operational environment, and production status is wayward, and direct labor's labour intensity is bigger.The 2nd, carburising step is loaded down with trivial details, and difficulty is kept the balanced production of carbonation process, and carbonization time is long, and the carbonizing apparatus utilization ratio is low, causes the big defective of facility investment, more limits the above scale prodn of ton.The 3rd, add Wingdale in producing, the waste residue amount after the production increases, and even more serious is and caused secondary pollution.
The mother liquid of boric acid that utilizes salt acid system processing boron magnesium ore deposit to be discharged never is fully utilized.Mother liquid of boric acid, major ingredient magnesium chloride and hydrochloric acid, usually content of magnesium chloride is 34～38%, hydrochloric acid 1.2～2.1%.Be in the salt acid system processing boron magnesium ore deposit; Breeze is allocated to proper concn with mother liquor and water, used the salt acidolysis, generate and contain boric acid and magnesium chloride and small amount of hydrochloric acid solution; Because boric acid solubleness in magnesium chloride solution is less; So with the solution cooling, make temperature be reduced to 0-5 ℃ of temperature, separate out the boric acid crystallization, be the boric acid finished product through spinning, drying.At present mother liquid of boric acid does not still have and rationally utilizes approach, discharging difficulty, contaminate environment.
Summary of the invention
The objective of the invention is provides a kind of technology more reasonable to above-mentioned deficiency, and refuse makes full use of, and is fit to the above scale prodn of ton, and the boron mud that utilizes that production efficiency is high is produced the method for magnesium basic carbonate.
Technical solution of the present invention is: utilize boron mud to produce the method for magnesium basic carbonate, its step is following:
(1) boron mud drying treatment: boron mud is carried out automatic drying handle under 160～280 ℃ of temperature, it is subsequent use to process boron mud powder again.
(2) batching: the hot water and the mother liquid of boric acid of boron mud powder and 80 ℃～85 ℃ were mixed with slip by weight 1: 1.5: 1.5; Being heated with stirring to 95～100 ℃ simultaneously handled 30～45 minutes; Adopt 80 ℃～85 ℃ hot water to be beneficial to and heat, reduce this step warm-up time.Hot water can be used the mother liquor water that discharges after the press filtration of this technology here, and circulation is squeezed into, and has promptly utilized the production hot wastewater, recycles, and waste and old utilization can also realize continuous production, water saving.Mother liquid of boric acid: content of magnesium chloride is 34～38%, hydrochloric acid 1.2～2.1%.
(3) size mixing: the slip for preparing is squeezed in the jar of sizing mixing; Add cold water (being generally underground water) below 15 ℃ simultaneously and reduce the concentration and the temperature of slip; Keep degree Beaume Be ' 2.4～2.2,20～30 ℃ of temperature, the slip that mixes up concentration is subsequent use in the jar of sizing mixing.In the jar of sizing mixing, size mixing, the ratio of sizing mixing is controlled easily, also can reduce carbonizing apparatus, and the carbonizing apparatus turnover rate is high, is convenient to continuous production, boosts productivity.Mother liquid of boric acid in the batching contains hydrochloric acid, can also serve as catalyst action.
(4) carbonization: subsequent use slip is squeezed in the carbonization jar in due order continuously in the jar of will sizing mixing, and uses CO
2The kiln gas carbonization of content 30%～33%, pressure-controlling are at 0.55～0.6MPa, and in 1.5～3 hours reaction times, temperature is controlled 25～32 ℃ or normal temperature, stopped reaction when being zero according to two gas differences.
(5) filter: carbodiimide solution is squeezed into Plate Filtration get filtrating and obtain heavy magnesium water, dry up body refuse, make moisture 30% left and right sides body refuse specify stacking, be used to process little fertilizer and brickmaking with carbonization tail gas.
(6) pyrolysis: its heavy magnesium water is squeezed in the pyrolysis tower, carried out thermolysis with 0.4Mpa steam, temperature is controlled at 95～100 ℃ and kept 15～20 minutes.
(7) press filtration: pyrolysis liquid is squeezed into flame filter press with pump, and dry up filter cake, can obtain moisture about 70% work in-process filter cake with carbonization tail gas.Filtrating (mother liquor water) treated turn back to the batching and the operation of sizing mixing recycle.
(8) drying: with moisture about 70% filter cake, be controlled at the drying machine temperature and carry out drying below 150 ℃, magnesium basic carbonate.
Preferably utilize boron mud to produce the method for magnesium basic carbonate, its step is following:
(1) boron mud drying treatment: boron mud is carried out automatic drying handle under 160～280 ℃ of temperature, it is subsequent use to process boron mud powder again;
(2) batching: boron mud powder and 80 ℃ hot water (or mother liquor water) and mother liquid of boric acid were mixed with slip by weight 1: 1.5: 1.5, are heated with stirring to 95～100 ℃ of processing simultaneously and sent into afterwards the jar of sizing mixing in 30～45 minutes.
(3) size mixing: the slip for preparing is squeezed in the jar of sizing mixing, added concentration and temperature that cold water below 15 ℃ reduces slip simultaneously, keep degree Beaume Be ' 2.4～2.2,25 ℃ of temperature, the slip that mixes up concentration is subsequent use in the jar of sizing mixing;
(4) carbonization: subsequent use slip is squeezed in the carbonization jar in due order continuously in the jar of will sizing mixing, and uses CO
2The kiln gas carbonization of content 30%, pressure-controlling be at 0.55～0.6MPa, 2 hours reaction times, normal temperature, stopped reaction when being zero according to two gas differences;
(5) filter: carbodiimide solution is squeezed into Plate Filtration get filtrating and obtain heavy magnesium water;
(6) pyrolysis: its heavy magnesium water is squeezed in the pyrolysis tower, carried out thermolysis with 0.4Mpa steam, temperature is controlled at 95～100 ℃, keeps 15～20 minutes;
(7) press filtration: pyrolysis liquid is squeezed into flame filter press with pump, and dry up filter cake, can obtain moisture about 70% work in-process filter cake with carbonization tail gas;
(8) drying: with the work in-process filter cake, be controlled at the drying machine temperature and carry out drying below 150 ℃, magnesium basic carbonate.
More than the main chemical reactions of getting in each process step of magnesium basic carbonate by boric sludge following:
1. boron mud is handled
2. batching is handled
3. the carbonization of sizing mixing
4. thermolysis
Advantage of the present invention is: 1, boron mud is handled through whizzer automatically; Need not press the brick roasting also can produce magnesium basic carbonate, also solve in the production process simultaneously, direct labor's labour intensity is big; Severe operational environment, production status is wayward and influence the disadvantage of carbonization because of roasting quality.2, utilized the difficult mother liquid of boric acid of discharging to prepare burden.The mother liquid of boric acid that the present invention adds not only can water saving, improves processing condition, can also utilize the effective constituent in the mother liquid of boric acid, is enough to play catalyst action, improves the yield of magnesium basic carbonate.3, set up the operation of sizing mixing, solved in the carbonization jar and diluted in the operating process of slip, be difficult to guarantee that the needed slip of carbonization reaches requirement concentration, and be difficult to keep the difficult problem of carbonization jar balanced production, can improve the yield of product greatly with cold water.Setting up of the operation of sizing mixing is for the scale prodn more than the ton with enlarge to produce and lay a good foundation.4, carbonization time shortens half thely, has improved plant factor, and it is nearly about 30% to have reduced facility investment, is fit to extensive chemical industry production, significantly energy-conservation with shorten the production cycle, and can produce high-quality magnesium basic carbonate and multiple product.Reduce water consumption 25%.5, the waste residue amount is few in the production process, can produce the required little fertilizer of the ecological agriculture and non-burning brick with waste residue, has reached zero release, has protected environment.
To combine embodiment that embodiment of the present invention is described in further detail below.
Embodiment
Embodiment 1
Utilize boron mud to produce the method for magnesium basic carbonate: to add 85 ℃ of hot water 1500Kg (or 1.5M toward the 1# material-compound tank
3) again, add mother liquid of boric acid 1500Kg (or 1.5M
3), start stirrer then, drop into the boron mud powder 1000Kg that drying treatment is crossed; And ℃ handled 30 minutes with steam direct heating to 98, sealing feeds intake and draws port lid, with the tail gas pressurization this slip is pressed into 1# and sizes mixing in the jar; Start stirring and add 13 ℃ underground cold water simultaneously to 2.4Be ' time, close water supply valve and stop to add water, at this moment testing slurry temperature is 24 ℃; Start steam piano then this slip is squeezed in the 7# carbonization jar, then feed CO
232%, pressure-controlling is at 0.55～0.6Mpa, and having reacted 2.5 hours survey two gas differences is the zero reaction that stopped; With tail gas pressurization this carbonization jar slip is got filtrating through Plate Filtration, squeezes into 1# pyrolysis tower, with the 0.4Mpa steam heating 43 minutes temperature to 100 ℃; After having kept 15 minutes, squeeze into the secondary filtration plate-and-frame filter press with pump, tail gas dries up filter cake after 23 minutes; At this moment back out filter plate and obtain moisture 72% filter cake, after drying treatment, get dry product 328.4Kg.
Embodiment 2
Utilize boron mud to produce the method for magnesium basic carbonate: to add 80 ℃ of mother liquor water 1500Kg toward the 2# material-compound tank, add mother liquid of boric acid 1500Kg again, start stirrer then; Drop into the boron mud powder 1000Kg that drying treatment is crossed, and ℃ handled 35 minutes, stop to stir that sealing feeds intake draws port lid with steam direct heating to 96; With tail gas pressurization this slip is pressed into 2# and sizes mixing in the jar, start stirring and add 13 ℃ underground cold water simultaneously, close water valve and stop to add water to 2.4Be ' time; At this moment testing slurry temperature is 25 ℃; Start steam piano then, this slip is squeezed in the 8# carbonization jar, then feed 32%CO
2Pressure-controlling is at 0.55～0.6Mpa, and having reacted 3 hours survey two gas differences is the zero reaction that stopped, and with the tail gas pressurization this carbonization jar slip is got filtrating through Plate Filtration and squeezes into 2# pyrolysis tower; With the 0.4Mpa steam heating 40 minutes temperature to 100 ℃; After having kept 10 minutes, squeeze into plate-and-frame filter press with pump, tail gas dries up filter cake after 18 minutes; Back out filter plate and get moisture 71% filter cake, after drying treatment, get dry product 415Kg.
Embodiment 3
Utilize boron mud to produce the method for magnesium basic carbonate: to add 81 ℃ of mother liquor water (or water) 1500Kg toward the 1# material-compound tank, add mother liquid of boric acid 1500Kg again, start stirrer then; Drop into the boron mud powder 1000Kg that drying treatment is crossed, and after ℃ having handled 40 minutes with steam direct heating to 100, stop to stir that sealing feeds intake draws port lid; With tail gas pressurization this slip being pressed into 3# sizes mixing in the jar; Start stirring and add 13 ℃ underground cold water simultaneously to 2.4Be ' time, close water supply valve and stop to add water, at this moment testing slurry temperature is 26 ℃; Start steam piano then this slip is squeezed in the 9# carbonization jar, then feed 32%CO
2, pressure-controlling is at 0.55～0.6Mpa, and having reacted 2 hours 45 minutes survey two gas differences is the zero reaction that stopped.With the tail gas pressurization this carbonization jar slip is got filtrating through Plate Filtration and squeeze into 3# pyrolysis tower; With the 0.4Mpa steam heating 50 minutes temperature to 100 ℃; After having kept 10 minutes, squeeze into plate-and-frame filter press with pump, tail gas dries up filter cake after 23 minutes; Back out filter plate and get moisture 70.4% filter cake, after drying treatment, get dry product 537Kg.
Product meets national GB161298 top grade article standard, its index such as table 1 through detecting:
Table 1 product detects index
Claims (1)
1. method of utilizing boron mud to produce magnesium basic carbonate, its step is following:
(1) boron mud drying treatment: boron mud is carried out automatic drying handle under 160～280 ℃ of temperature, it is subsequent use to process boron mud powder again;
(2) batching: boron mud powder and 80 ℃～85 ℃ hot water and mother liquid of boric acid are mixed with slip by weight 1:1.5:1.5, are heated with stirring to 95～100 ℃ of processing 30～45 minutes simultaneously, send into the jar of sizing mixing;
(3) size mixing: the slip for preparing is squeezed in the jar of sizing mixing, added concentration and temperature that cold water below 15 ℃ reduces slip simultaneously, keep degree Beaume Be ' 2.4～2.2,20～30 ℃ of temperature, the slip that mixes up concentration is subsequent use in the jar of sizing mixing;
(4) carbonization: subsequent use slip is squeezed in the carbonization jar in due order continuously in the jar of will sizing mixing, and uses CO
2The kiln gas carbonization of content 30%～33%, pressure-controlling are at 0.55～0.6MPa, and in 1.5～3 hours reaction times, temperature is controlled 25～32 ℃ or normal temperature, stopped reaction when being zero according to two gas differences;
(5) filter: carbodiimide solution is squeezed into Plate Filtration get filtrating and obtain heavy magnesium water;
(6) pyrolysis: its heavy magnesium water is squeezed in the pyrolysis tower, carried out thermolysis with 0.4Mpa steam, temperature is controlled at 95～100 ℃, keeps 15～20 minutes;
(7) press filtration: pyrolysis liquid is squeezed into flame filter press with pump, and dry up filter cake, obtain moisture 70% work in-process filter cake with carbonization tail gas;
(8) drying: with the work in-process filter cake, be controlled at the drying machine temperature and carry out drying below 150 ℃, magnesium basic carbonate.
2, according to the described method of utilizing boron mud to produce magnesium basic carbonate of claim 1, it is characterized in that step is following:
(1) boron mud drying treatment: boron mud is carried out automatic drying handle under 160～280 ℃ of temperature, it is subsequent use to process boron mud powder again;
(2) batching: boron mud powder and 80 ℃ hot water and mother liquid of boric acid are mixed with slip by weight 1:1.5:1.5, are heated with stirring to 95～100 ℃ of processing 30～45 minutes simultaneously, send into the jar of sizing mixing;
(3) size mixing: the slip for preparing is squeezed in the jar of sizing mixing, added concentration and temperature that cold water below 15 ℃ reduces slip simultaneously, keep degree Beaume Be ' 2.4～2.2,25 ℃ of temperature, the slip that mixes up concentration is subsequent use in the jar of sizing mixing;
(4) carbonization: subsequent use slip is squeezed in the carbonization jar in due order continuously in the jar of will sizing mixing, and uses CO
2The kiln gas carbonization of content 30%, pressure-controlling be at 0.55～0.6MPa, 2 hours reaction times, normal temperature, stopped reaction when being zero according to two gas differences;
(5) filter: carbodiimide solution is squeezed into Plate Filtration get filtrating and obtain heavy magnesium water;
(6) pyrolysis: its heavy magnesium water is squeezed in the pyrolysis tower, carried out thermolysis with 0.4Mpa steam, temperature is controlled at 95～100 ℃, keeps 15～20 minutes;
(7) press filtration: pyrolysis liquid is squeezed into flame filter press with pump, and dry up filter cake, obtain moisture 70% work in-process filter cake with carbonization tail gas;
(8) drying: with the work in-process filter cake, be controlled at the drying machine temperature and carry out drying below 150 ℃, magnesium basic carbonate.
3, a kind of method of utilizing boron mud to produce magnesium basic carbonate is characterized in that step is following:
Add 81 ℃ of mother liquor water 1500Kg toward the 1# material-compound tank, add mother liquid of boric acid 1500Kg again, start stirrer then; Drop into the boron mud powder 1000Kg that drying treatment is crossed, and after ℃ having handled 40 minutes with steam direct heating to 100, stop to stir that sealing feeds intake draws port lid; With tail gas pressurization this slip being pressed into 3# sizes mixing in the jar; Start stirring and add 13 ℃ underground cold water simultaneously to 2.4Be ' time, close water supply valve and stop to add water, at this moment testing slurry temperature is 26 ℃; Start steam piano then this slip is squeezed in the 9# carbonization jar, then feed 32%CO
2, pressure-controlling is at 0.55～0.6Mpa, and having reacted 2 hours 45 minutes survey two gas differences is the zero reaction that stopped; With the tail gas pressurization this carbonization jar slip is got filtrating through Plate Filtration and squeeze into 3# pyrolysis tower; With the 0.4Mpa steam heating 50 minutes temperature to 100 ℃; After having kept 10 minutes, squeeze into plate-and-frame filter press with pump, tail gas dries up filter cake after 23 minutes; Back out filter plate and get moisture 70.4% filter cake, after drying treatment, get dry product 537Kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102531586A CN102320633B (en) | 2011-08-31 | 2011-08-31 | Method for producing basic magnesium carbonate by boron sludge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102531586A CN102320633B (en) | 2011-08-31 | 2011-08-31 | Method for producing basic magnesium carbonate by boron sludge |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102320633A CN102320633A (en) | 2012-01-18 |
| CN102320633B true CN102320633B (en) | 2012-08-01 |
Family
ID=45448513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102531586A Expired - Fee Related CN102320633B (en) | 2011-08-31 | 2011-08-31 | Method for producing basic magnesium carbonate by boron sludge |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102320633B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104418573A (en) * | 2013-08-22 | 2015-03-18 | 丹东玉龙镁业有限公司 | Method for comprehensive utilization of industrial waste boron sludge |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944259A (en) * | 2006-11-03 | 2007-04-11 | 高佳令 | Process for producing industrial magnesium oxide using dolomite ash and boron mud |
| CN101077781A (en) * | 2007-07-02 | 2007-11-28 | 高佳令 | Technique for separating boron and magnesium from ascharite |
| CN101683988A (en) * | 2008-09-23 | 2010-03-31 | 东北大学 | Method for producing series magnesia chemical products by using material containing magnesium |
-
2011
- 2011-08-31 CN CN2011102531586A patent/CN102320633B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944259A (en) * | 2006-11-03 | 2007-04-11 | 高佳令 | Process for producing industrial magnesium oxide using dolomite ash and boron mud |
| CN101077781A (en) * | 2007-07-02 | 2007-11-28 | 高佳令 | Technique for separating boron and magnesium from ascharite |
| CN101683988A (en) * | 2008-09-23 | 2010-03-31 | 东北大学 | Method for producing series magnesia chemical products by using material containing magnesium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102320633A (en) | 2012-01-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106892437B (en) | Utilize the preparation method of pumice synthetic zeolite | |
| CN110982547A (en) | Method for reducing strong basicity of red mud | |
| CN103803584B (en) | Ammonium bifluoride preparation method | |
| CN101633981B (en) | Titaniferous material acidolysis method and titanium dioxide preparing method | |
| CN108728899B (en) | Method for preparing high-purity calcium carbonate whiskers by pressurizing, injecting and mixing circulating mother liquor | |
| CN109824072A (en) | The method for preparing aluminium oxide using industrial residue | |
| CN102295441A (en) | Aerated concrete brick produced by using tailing slags | |
| CN111908876A (en) | Production and processing method of high-strength autoclaved sand-lime brick | |
| CN105129852B (en) | The system that a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate | |
| CN102531423A (en) | Method for producing cement clinker by utilizing red mud | |
| CN102701220A (en) | Method for preparing white carbon black by oxygen-free high-temperature calcination and thermal activation of coal gangue | |
| CN101704556B (en) | Method and system for continuous production of potassium manganate by low-grade pyrolusite | |
| CN102503190A (en) | Method and device for preparing high-purity high-density magnesia by utilizing magnesite | |
| CN102320633B (en) | Method for producing basic magnesium carbonate by boron sludge | |
| CN102372620B (en) | Magnesium Stearate improves the preparation method of its specific volume and whiteness | |
| CN101367554B (en) | Method for preparing potassium manganate solution | |
| CN104262991B (en) | A kind of method of semi-continuous production white dyes | |
| CN107117630B (en) | A method of roasting illite efficiently carries potassium | |
| CN102336416B (en) | Method for cleanly producing high-purity cyanate at low temperature | |
| CN101817204A (en) | Production flow line of acid-resistant, high temperature-resistant and high pressure-resistant earthenware brick | |
| CN107010852B (en) | A kind of light calcined magnesia production method | |
| CN201932918U (en) | Device for producing nano calcium carbonate by using quicklime | |
| CN206705693U (en) | A kind of system for preparing calcium carbide smelting palletizing using carbide slag and lignite | |
| CN204198436U (en) | A kind of continous way digestion reaction device preparing Magnesium Carbonate Light 41-45 | |
| CN115924953B (en) | Method for producing ultrahigh-strength gypsum by using waste residue gypsum liquid phase method and gypsum |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120801 Termination date: 20150831 |
|
| EXPY | Termination of patent right or utility model |