CN101279738B - Liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction - Google Patents
Liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction Download PDFInfo
- Publication number
- CN101279738B CN101279738B CN2008100615087A CN200810061508A CN101279738B CN 101279738 B CN101279738 B CN 101279738B CN 2008100615087 A CN2008100615087 A CN 2008100615087A CN 200810061508 A CN200810061508 A CN 200810061508A CN 101279738 B CN101279738 B CN 101279738B
- Authority
- CN
- China
- Prior art keywords
- phase reaction
- liquid phase
- staving
- tube
- reaction pot
- 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
Abstract
The invention discloses a liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction, comprising a barrel, a feeding tube, a vent tube, a sampling tube and a reclaiming tube. A double-layer mixing stirring paddle is arranged in the barrel. A pressure gauge, a safety valve, the feeding tube, the vent tube and the sampling tube are arranged in an upper end head of the barrel. The reclaiming tube is arranged along a lower end head wall to the lowest point of the barrel at the position near the lower end head from the barrel. The reclaiming tube is simultaneously used as a steam tube. The invention has simple device structure, convenient operation, low investment, fast effect, and no "three waste" generation during the use process, which is a green environmental protection novel device.
Description
Technical field
The present invention relates to a kind of preparation method of liquid sodium silicate, particularly a kind of method of utilizing liquid phase reaction to prepare liquid sodium silicate.
Background technology
Traditional water glass production technique is that quartz sand and soda ash are dropped in the special-purpose high-temperature roasting stove, and with coal or oily heating and melting, blowing behind the sufficient reacting directly washes chilling with cold water during discharging, forms glassy water glass solid piece.Utilize the fusion cylinder that this piece water and a certain amount of liquid caustic soda are pressurized to 0.6-0.7Mpa again and fuse into the liquid sodium silicate product.There are many problems in this method:
1. dioxide-containing silica is generally 95-97% in the quartz sand ore, contain metal ions such as a large amount of iron, calcium, magnesium, aluminium, after high-temperature roasting, these ions and water glass form the poly material of fritting, it can't effectively be separated with finished product, contain a large amount of impurity in the back road product.Water glass after the fusion can only use the less demanding industrialness of impurity as adhesive for paper box or ceramic dispersants etc., can't use as further chemosynthesis product.
2. will make piece that liquid sodium silicate also must come out stoving oven and add alkali again and add the water reaction under high pressure, technological process is long, consumes a large amount of energy, is unfavorable for national industrial policies.
3. can only produce relatively single product.Stoving oven come out finished product SiO
2And Na
2O ratio (modulus) generally can only be accomplished 3.2M-3.6M.Also must add a set of equipment in actual the use in addition is used for regulating.
4. the investment of stoving oven and high pressure roller equipment is big, and floor space is many, is non-standard equipment, and control also is difficult for.
Quality product criticize the difference bigger, be unfavorable for industrial production control.
Summary of the invention
The invention provides a kind of method of utilizing the single stage method liquid phase reaction to prepare liquid sodium silicate, change former solid phase method and produce the method for liquid sodium silicate, adopt and directly quartz sand and liquid caustic soda are reacted in specific liquid phase reaction pot, in control rational temperature, pressure and the reaction times, obtain best transformation efficiency and product quality.
The present invention also provides a kind of liquid phase reaction pot that is exclusively used in this method.
A kind of method of utilizing the single stage method liquid phase reaction to prepare liquid sodium silicate comprises: with quartz sand and liquid caustic soda with SiO
2: NaOH mol ratio 2.2-3.4: 1 mixes, whipped state is pumped into this mixture in the liquid phase reaction pot of opening stirring down, directly feed steam heating, treat to stop when pot inner pressure reaches 0.65Mpa steam, automatically boost to 0.65-0.75Mpa, fully reacted step-down 4-6 hour, carry out vacuum filtration, getting filtrate is liquid sodium silicate.The quartz sand transformation efficiency can be 92%-95%, and the liquid caustic soda transformation efficiency can be 100%.
Described quartz sand is selected SiO for use
2The quartz sand of content more than 99.0%.Common quartz sand SiO
2Content generally has only 95-96%, contains metal complex ions such as relatively large iron, calcium, aluminium, magnesium, and under above-mentioned reaction conditions, easy and alkali reaction makes to occur a large amount of impurity in the product, handles for the road, back and increases pressure, and make quality of finished decline.SiO
2The quartz sand of content more than 99.0%, outward appearance is pure white, and metal ion content is below 0.7%, thereby guaranteed quality of finished.
Described liquid caustic soda is selected diaphragm caustic soda or ionic membrane caustic soda for use, and content is 30% GB.
A kind of liquid phase reaction pot that is exclusively used in aforesaid method comprises staving, feed-pipe, blow-down pipe, stopple coupon and discharge nozzle, is provided with double-deck stirring arm in the described staving; Be provided with tensimeter, safety valve, feed-pipe, blow-down pipe and stopple coupon in the upper cover of staving, tensimeter test staving internal pressure, for guaranteeing safety, can be provided with two, can use second during a damage, during step-down, steam is discharged by blow-down pipe, and the steam of discharging can be led to another liquid phase reaction pot preheating; Be provided with discharge nozzle along the lower cover wall to the staving lower-most point near the lower cover place from staving in the staving, discharge nozzle is simultaneously as the pipeline that feeds steam.
Described staving can be provided with man-hole opening, makes things convenient for internal examination and maintenance; Select for use the 16Mn steel as material, increase the wear resistance of bucket wall, prolong the reactor life-span; The staving height is 1 with the diameter ratio: 2.2-2.3 helps liquid-solid reaction thoroughly to carry out.
The paddle of described double-deck stirring arm guarantees thorough mixing, the reaction of staving internal reaction material apart from staving inwall 25-40mm.
Described stopple coupon extends to the staving mid-way along the bucket wall in upper cover stretches into staving.
Described staving is provided with thermal insulation layer outward, and thermal insulation layer adopts the insulating rare earth composite material.
The present invention has the following advantages:
1. synthetic route is short, and the reference mark is few, and is simple to operate;
2. production site is little, and the liquid phase reaction pot can directly stand on ground, and construction investment economizes;
3. need not stoving oven, the contour energy consumption equipment of high pressure roller, the production process energy consumption is low, high efficiency;
4. facility investment not until old 1/5 of technology, reduced investment, instant effect;
5. with respect to old technology, liquid sodium silicate product foreign matter content of the present invention descends more than 90%, and from having promoted the product quality of liquid sodium silicate in essence, thereby developing water glass product is in the application of every field.Particularly, in free phosphate detergent, replace phosphoric acid salt to bring into play enormous function as derived product (Starso, sodium metasilicate etc.).
6. production unit can not wait from the 1-30 cubic meter, and investment and industrial scale are controlled easily;
7. can be with a plurality of liquid phase reaction pots, waste heat can be used as another reactor preheating usefulness during step-down, does not waste heat energy.
8. reaction mass utilizes overbottom pressure to deliver to voluntarily in the suction filtration bucket, need not pumping;
9. can produce the purpose product of different moduluses when preparing burden according to the quartz sand and the different ratios of liquid caustic soda, the equipment suitability is strong;
10. reaction process only need be controlled liquid material pressure, need not control reaction temperature;
11. can increase or the minimizing reaction times according to raw material is different, reach the ideal reaction efficiency;
12. the sand slag behind the vacuum filtration can return batching and reuse, and neither wastes raw material, and waste residue also do not occur;
Do not produce 13. whole process of production has " three wastes ", belong to " green chemical industry " production technology.
Description of drawings
Fig. 1 is the structural representation of liquid phase reaction pot.
Embodiment
Further specify preferred forms of the present invention below in conjunction with the drawings and specific embodiments, but the present invention is not limited to this.
Design 12 cubic metres of liquid phase reaction pots, make staving 1 with thick 16 manganese steel plates of 14cm and corresponding standard sealing head, staving 1 diameter 1800mm, virtual height 4000mm respectively establishes a man-hole opening 9 up and down at staving 1.
Be provided with double-deck stirring arm 6 in the staving 1, stirring blade is apart from bucket inwall 30mm; Be provided with a feed-pipe 2, two tensimeters 7, blow-down pipe 3, a safety valve 8 (0.75Mpa) and a stopple coupon 4 in the upper cover, stopple coupon 4 extends to staving 1 mid-way along a bucket wall in upper cover stretches into staving 1; 1 lower-most point is provided with discharge nozzle 5 along the lower cover wall to staving near the lower cover place from staving 1 in the staving 1, and discharge nozzle 5 is convenient to homogeneous heating simultaneously as the pipeline that feeds steam, and discharging is clean.
For avoiding calorific loss, the insulation of entire reaction pot.Thermal insulation layer adopts the insulating rare earth composite material, the suitable 17-20cm of thermal insulation layer, and heat insulation effect is good.
Embodiment 1
In ingredients pot with SiO
2Anhui product No. seven quartz sands and 30% liquid caustic soda of content more than 99% mixes with mol ratio at 2.45: 1, whipped state is pumped into this mixture in the liquid phase reaction pot of opening stirring down, directly feed steam heating, treat to stop when pot inner pressure reaches 0.65Mpa steam, automatically boost to 0.7Mpa, fully reaction is 4 hours, sampling analysis, when modulus reaches 2.4M, by blow-down pipe steam in the reactor is discharged step-down, it is interior as preheating usefulness that the steam of discharge leads to another reactor, treats that pressure drops to 0.3Mpa, put into the suction filtration bucket and carry out vacuum filtration, the filtrate that obtains is the 2.4M liquid sodium silicate of purity more than 99.0%.
Embodiment 2:
In ingredients pot with SiO
2Anhui product No. seven quartz sands and 30% liquid caustic soda of content more than 99% mixes with mol ratio at 3.25: 1, whipped state is pumped into this mixture in the liquid phase reaction pot of opening stirring down, directly feed steam heating, treat to stop when pot inner pressure reaches 0.65Mpa steam, automatically boost to 0.7Mpa, fully reaction is 5.5 hours, sampling analysis, modulus reaches 3.2M, by blow-down pipe steam in the reactor is emitted step-down, it is interior as preheating usefulness that the steam of emitting feeds another reactor, treats that pressure drops to 0.3Mpa, put into the suction filtration bucket and carry out vacuum filtration, suction filtration liquid material is the 3.2M liquid sodium silicate of purity more than 99.0%.
Claims (6)
1. a liquid phase reaction pot that utilizes the single stage method liquid phase reaction to prepare liquid sodium silicate comprises staving (1), feed-pipe (2), blow-down pipe (3), stopple coupon (4) and discharge nozzle (5), is provided with double-deck stirring arm (6) in the described staving; Be provided with tensimeter (7), safety valve (8), feed-pipe (2), blow-down pipe (3) and stopple coupon (4) in the upper cover of staving (1); (1) lower-most point is provided with discharge nozzle (5) along the lower cover wall to staving near the lower cover place from staving (1) in the staving (1), and described discharge nozzle (5) is simultaneously as the pipeline that feeds steam.
2. liquid phase reaction pot as claimed in claim 1 is characterized in that: described staving (1) is provided with man-hole opening (9).
3. liquid phase reaction pot as claimed in claim 1 or 2 is characterized in that: described staving (1) selects for use 16 manganese steel as material, and staving (1) height is 1 with the diameter ratio: 2.2-2.3.
4. liquid phase reaction pot as claimed in claim 1 is characterized in that: the paddle of described double-deck stirring arm (6) is apart from bucket inwall 25-40mm.
5. liquid phase reaction pot as claimed in claim 1 is characterized in that: described stopple coupon (4) extends to the interior mid-way of staving (1) along the bucket wall.
6. liquid phase reaction pot as claimed in claim 1 is characterized in that: the outer thermal insulation layer that is provided with of described staving (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100615087A CN101279738B (en) | 2008-05-12 | 2008-05-12 | Liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100615087A CN101279738B (en) | 2008-05-12 | 2008-05-12 | Liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101279738A CN101279738A (en) | 2008-10-08 |
| CN101279738B true CN101279738B (en) | 2011-12-21 |
Family
ID=40012445
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100615087A Expired - Fee Related CN101279738B (en) | 2008-05-12 | 2008-05-12 | Liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101279738B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101518724B (en) * | 2009-03-27 | 2012-01-11 | 张新军 | Self-adjusting quick reaction kettle |
| CN102153099A (en) * | 2010-12-15 | 2011-08-17 | 何侠 | Method for preparing water glass and hydrophobic silicon dioxide by using treatment waste slag of calcined sulfate slag |
| CN102153100A (en) * | 2010-12-15 | 2011-08-17 | 何侠 | Method for preparing water glass and electronic silicon dioxide from treatment waste residues of sulfuric acid slags |
| CN103754890A (en) * | 2013-12-17 | 2014-04-30 | 柳州东风化工股份有限公司 | Preparation method for anhydrous sodium metasilicate |
| CN103738973A (en) * | 2013-12-17 | 2014-04-23 | 柳州东风化工股份有限公司 | Preparation method of sodium metasilicate pentahydrate |
| CN104118880B (en) * | 2014-07-02 | 2016-01-20 | 广州立白企业集团有限公司 | A kind of wet production sodium silicate automatic blending Processes and apparatus |
| CN104261419B (en) * | 2014-10-14 | 2016-05-25 | 龙星化工股份有限公司 | A kind of production method of liquid sodium silicate |
| US11667534B2 (en) | 2018-05-25 | 2023-06-06 | Agripower Australia Limited | Method for extracting soluble Si from an amorphous SiO2 bearing material |
| AU2019381854A1 (en) * | 2018-11-16 | 2021-06-10 | Cotton Research And Development Corporation | Alkaline digestion of glass |
| CN109395673B (en) * | 2018-12-01 | 2021-08-10 | 山东龙港硅业科技有限公司 | Continuous liquid phase reactor and process method for producing liquid sodium silicate by using same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0033108A1 (en) * | 1980-01-26 | 1981-08-05 | Henkel Kommanditgesellschaft auf Aktien | Process for the hydrothermal production of sodium silicate solutions |
| US4770866A (en) * | 1984-06-07 | 1988-09-13 | Henkel Kommanditgesellschaft Auf Aktien | Hydrothermal production of clear sodium silicate solutions |
| CN1044632A (en) * | 1989-01-31 | 1990-08-15 | 亨克尔两合股份公司 | The method of hydrothermal preparating solution of solidum silicate |
| CN1051897A (en) * | 1989-11-23 | 1991-06-05 | 亨克尔两合股份公司 | The method of process for preparation of solution of potassium silicate by hydrothermal |
| CN2563157Y (en) * | 2002-07-05 | 2003-07-30 | 兖矿科蓝煤焦化有限公司 | Impregnant asphalt beta resin reactor |
-
2008
- 2008-05-12 CN CN2008100615087A patent/CN101279738B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0033108A1 (en) * | 1980-01-26 | 1981-08-05 | Henkel Kommanditgesellschaft auf Aktien | Process for the hydrothermal production of sodium silicate solutions |
| US4770866A (en) * | 1984-06-07 | 1988-09-13 | Henkel Kommanditgesellschaft Auf Aktien | Hydrothermal production of clear sodium silicate solutions |
| CN1044632A (en) * | 1989-01-31 | 1990-08-15 | 亨克尔两合股份公司 | The method of hydrothermal preparating solution of solidum silicate |
| CN1051897A (en) * | 1989-11-23 | 1991-06-05 | 亨克尔两合股份公司 | The method of process for preparation of solution of potassium silicate by hydrothermal |
| CN2563157Y (en) * | 2002-07-05 | 2003-07-30 | 兖矿科蓝煤焦化有限公司 | Impregnant asphalt beta resin reactor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101279738A (en) | 2008-10-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101279738B (en) | Liquid phase reaction pot for preparing liquid sodium silicate by one-step liquid phase reaction | |
| KR20110076565A (en) | Vertical type thermal reduction apparatus for magnesium production and method for magnesium production by its apparatus | |
| CN102584294A (en) | Composite fire-proof material with high refractoriness under load for coke ovens as well as furnace-building process and products thereof | |
| CN103553501B (en) | The preparation method of calcium-silicate thermal insulation material | |
| CN101999005A (en) | Vacuum circulation molten state silicothermic method for producing magnesium and equipment thereof | |
| CN102583389A (en) | Method for purifying industrial silicon through external refining | |
| CN201713555U (en) | Combined type refining furnace for continuously producing mixed cropper regeneration casting anode plates | |
| CN101906544A (en) | Double-dip pipe ferrosilicon bath vacuum circular flow magnesium-smelting device and method thereof | |
| CN101914692B (en) | Single-dip pipe silicon iron bath vacuum circulated magnesium-smelting device and method | |
| CN107141001A (en) | Compound fibre reinforced iron runner castable | |
| CN103993116B (en) | Double tower flash iron-smelting furnace and iron smelting method | |
| CN101215180B (en) | Method for producing AZS electric melting refractory materials by natural mineral raw materials | |
| CN105002371A (en) | Process for producing anode copper by adoption of four connected furnaces | |
| CN101318121A (en) | Reaction tank for producing flocculating agent | |
| CN102898151A (en) | Iron-storage type casting material for iron tapping channel, and preparation method thereof | |
| CN102815715B (en) | Method for producing electronic mica via artificial synthesis | |
| CN105777158A (en) | Siliceous dry material for tundish for steel smelting as well as production method and construction method | |
| CN110981449A (en) | Steel ladle pocket brick thermal-state repairing material and preparation method thereof | |
| CN1459345A (en) | New type tundish dry working liner | |
| CN106495172A (en) | The method that xonotlite fiber is produced using sour solution-off aluminium powder coal ash and carbide slag | |
| CN201842881U (en) | Vacuum reduction equipment for directly producing magnesium from magnesite in one-step method | |
| CN105294071A (en) | Lining type container used for precious metal crucible and preparation method thereof | |
| CN105174982B (en) | Preparation method for the castable of blast furnace tuyere small sleeve and its with tuyere small sleeve | |
| CN102010005A (en) | Method for preparing chromic oxide | |
| CN2883385Y (en) | NOvel assembling methane tank |
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 | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111221 Termination date: 20140512 |