CN103466637A - Method for producing precipitate silicon dioxide by using sodium bicarbonate to control supersaturation degree - Google Patents
Method for producing precipitate silicon dioxide by using sodium bicarbonate to control supersaturation degree Download PDFInfo
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- CN103466637A CN103466637A CN2013103828940A CN201310382894A CN103466637A CN 103466637 A CN103466637 A CN 103466637A CN 2013103828940 A CN2013103828940 A CN 2013103828940A CN 201310382894 A CN201310382894 A CN 201310382894A CN 103466637 A CN103466637 A CN 103466637A
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Abstract
A method for producing precipitate silicon dioxide by using sodium bicarbonate to control a supersaturation degree comprises the steps of taking quartz sand and soda as raw materials, roasting, dissolving a sodium carbonate solution to prepare a sodium silicate solution, allowing the sodium silicate solution to react with a sodium bicarbonate solution, separating out a hydrated silicon dioxide precipitate by a method for controlling the reaction crystallization supersaturation degree, washing and drying the filtered precipitate, and finally obtaining precipitate silicon dioxide, namely white carbon black. Filtered filtrate is the sodium carbonate solution which is recycled for absorbing carbon dioxide from a roasting working section to prepare a concentrated sodium bicarbonate solution required for crystallization reaction, dissolving solid sodium silicate, and returning to the quartz sand roasting working section after evaporation and concentration. Precipitate silicon dioxide prepared by the method is high in purity and uniform in particle size distribution; materials are recycled during the whole production flow; and the problem of sodium sulfate sewage discharge in conventional production is solved.
Description
Technical field
The invention belongs to the precipitated silica production field, particularly a kind of sodium silicate solution and sodium hydrogen carbonate solution of utilizing reacts, and controls degree of supersaturation by sodium hydrogen carbonate solution, the method for crystalline precipitated silica.
Background technology
Precipitated silica is commonly called as white carbon black, has another name called hydrated SiO 2, and molecular formula is SiO
2nH
2o, be a kind of white, nontoxic, unbodied super-fine powder, have porousness, polymolecularity, light weight, chemical stability good, high temperature resistant, do not burn and the excellent properties such as electrical insulating property is good.White carbon black is a kind of important Inorganic Chemicals, is widely used in the fields such as rubber, plastics, coating, papermaking, medicine, agricultural chemicals and daily-use chemical industry.The white carbon black in the whole world 70%, for rubber industry, is a kind of rubber reinforcing filler of excellent property at present.
The production method of white carbon black has two kinds of dry method and wet methods.Dry method comprises vapor phase process and arc process, and wet method comprises the precipitator method and gel method, wherein vapor phase process and precipitator method dominate in white carbon black production at home and abroad.Vapor phase process is mainly with SiCl
4for raw material, the product purity made is high, good dispersion degree, and particle is thin and spherical in shape, has excellent reinforcing property.But, due to the raw material costliness, the high and technical sophistication of production process energy consumption, make the application of vapor phase process in industry be restricted.The tradition precipitator method be take water glass as raw material, by the mineral acid acidifying, prepare white carbon black, the industrial sulfuric acid acidations that use more.With vapor phase process, compare, precipitator method raw material is easy to get, and the production process energy consumption is low, and flow process is simple, but the quality product made is lower, and in production process, has a large amount of sodium sulfate sewage to produce.
At present, some research workers improve traditional precipitator method technology.For example, document Quang, D.V.; Kim, J.-K.; Park, J.-K.; Park, S.-H.; Elineema, G.; Sarawade, P.B.; Kim, H.T., Effect of the gelation on the properties of precipitated silica powder produced by acidizing sodium silicate solution at the pilot scale.Chemical Engineering Journal2012,209,531-536. has reported a kind of production method of white carbon black.It is raw material that the method be take water glass and sulfuric acid, on the basis of traditional technology, by two step acid addings, controls gelation processes, and the recycling spray drying technology, by the Silicon dioxide, hydrate drying, obtains white carbon black product.Utilize the white carbon black grain size that the method obtains to be evenly distributed, there is higher specific surface area and pore volume, but and unresolved sodium sulfate effluent problem, this not only causes water resources and can utilize the waste of sodium sulfate resource, also produces serious environmental pollution.
Patent CN201110026112.0 discloses a kind of technique for preparing precipitated silica by the carbonic acid gas decomposition method.The method is usingd carbonic acid gas as precipitation agent, is passed in industrial metasilicate solution, obtains precipitated silica, and after precipitation, solution can be made into the sodium carbonate product of high added value, thereby eliminates sewage discharge.Patent CN200710062197.1 discloses a kind of method of preparing white carbon black from secondary carbon component, successively passes into CO twice in sodium silicate solution
2gas, adjust pH, realizes solid-liquid separation twice, and remaining sodium carbonate solution is made sodium hydroxide solution after causticization is concentrated.Patent CN201110267981.2 be take SILICA FUME as raw material, by the carborization synthesizing white carbon black, has realized the recycling of trade waste.Patent CN201110267968.7 proposes to take SILICA FUME as raw material, make water glass by sodium hydroxide thermokalite method, carry out carburizing reagent with carbonic acid gas again, in sodium carbonate raffinate after carbonization is filtered, add calcium hydroxide to carry out causticizing reaction, to have formed preparing white carbon black co-product calcium carbonate technology.These carbonization technology have all been avoided the unmanageable problem of large amount of sewage, but because the gas liquid reaction time is long, low conversion rate, and CO
2the mass transfer process complexity of gas in sodium silicate solution, be difficult to control effectively, thereby cause the precipitation size-grade distribution of acquisition inhomogeneous, and purity is not high, affects the industrial application of product.
Patent CN00132275.3 and patent CN02132723.8 propose to carry out the method for carburizing reagent in supergravity reactor, and Elevated Gravity has been strengthened mass-transfer progress, thereby has improved production efficiency, has shortened the production cycle.But the above-mentioned carbonic acid gas precipitator method all be take the technical grade water glass as raw material, require to use the higher sodium silicate solution of purity, and, when raw material impurity content is higher, can't produce qualified white carbon black product.
Patent CN200810048295.4 and patent CN201110078760.0 have been used ammonia precipitation method, and water glass is made to white carbon black with the ammonium bicarbonate soln reaction, and the gas produced in production process and filtrate, through recycle and reuse, have been realized the efficient utilization of raw material.Yet ammonium bicarbonate soln character is unstable, discharge CO easily decomposing more than 36 ℃
2and NH
3, precipitation process is wayward, makes the efficiency of precipitin reaction lower, the Granularity Distribution inequality.On the other hand, bicarbonate of ammonia and ammoniacal liquor is irritant smell and corrodibility all, be detrimental to health, and etching apparatus.
Summary of the invention
The objective of the invention is the deficiency existed for prior art, provide a kind of sodium hydrogen carbonate solution that utilizes to control degree of supersaturation, the method of crystalline precipitated silica, the precipitated silica product purity obtained is high, even particle size distribution, and whole Production Flow Chart Matter Transfer utilizes, and without waste liquid, produces.
The present invention is that to take quartz sand and soda ash be raw material, at first prepare sodium silicate solution through calcining, dissolving, again by water glass and reaction of sodium bicarbonate, separate out the hydrated SiO 2 precipitation by the method for controlling the reactive crystallization degree of supersaturation, filter the precipitation obtained and obtain the precipitated silica product through washing, drying.Filtrate after filtration is sodium carbonate solution, and by three part recycles: a part absorbs the carbonic acid gas that comes from calcining workshop section to prepare the required dense sodium hydrogen carbonate solution of crystallization reaction; A part is for dissolving solid-state water glass; Be back to quartz sand calcining workshop section after the last part evaporation concentration.
The reaction the present invention relates to has:
（1）SiO
2(s)+Na
2CO
3(s)=Na
2SiO
3(s)+CO
2(g)
（2）Na
2SiO
3(aq)+2NaHCO
3(aq)=SiO
2(s)+2Na
2CO
3(aq)+H
2O(aq)
（3）Na
2CO
3(aq)+CO
2(g)+H
2O(aq)=2NaHCO
3(aq)
The concrete technology step is as follows:
1) quartz sand and the solid-state water glass of soda ash calcining preparation
Selecting specification is 40～70 orders, SiO
2the quartz sand that content is 98.8%, prepare burden quartz sand and soda ash on request, and mole proportioning is 1:(1.2～1.8).Calcine 30～60min after mixing and obtain solid-state water glass under 1300～1400 ℃, reclaim CO simultaneously
2.
2) solid-state water glass dissolves
Solid-state water glass dissolves in sodium carbonate solution, obtains the sodium silicate solution that concentration is 1.2mol/L.
3) water glass and reaction of sodium bicarbonate crystallization
By step 2) resulting sodium silicate solution is placed in crystallization reactor, temperature is controlled at 40～50 ℃, turn on agitator, drip with peristaltic pump the sodium hydrogen carbonate solution that concentration is 2.7mol/L, control degree of supersaturation by drop rate and the dripping quantity of adjusting solution, separate out the hydrated SiO 2 precipitation.The concentration of above-mentioned temperature of reaction and reactant is conducive to the formation of crystal and separates out, thereby makes the crystallization purity of generation high, and crystal formation is better, has high specific surface area and pore volume, even particle size distribution.
4) prepare high-purity white carbon
By step 3) resulting suspension filtered, and obtains hydrated SiO 2 precipitation and sodium carbonate filtrate.Precipitation after filtration makes the precipitated silica product through washing, drying, pulverizing.
5) recycle of sodium carbonate solution
Step 4) the sodium carbonate filtrate obtained is divided three part recycles: the CO a part of sodium carbonate solution absorption step 1) obtained
2gas, control gas flow, obtains sodium hydrogen carbonate solution, turns back to step 3) recycle; Part sodium carbonate solution turns back to step 2), for dissolving solid-state water glass; The last part sodium carbonate solution, through evaporation concentration, turns back to step 1) calcined.
Advantage of the present invention and active effect are:
(1) the present invention utilizes sodium hydrogen carbonate solution to control degree of supersaturation, operating process is convenient, controllability is strong, and degree of supersaturation can directly affect the formation of nucleus and the growth of crystal as the motivating force of crystallization, and then affect granularity and the size-grade distribution of crystal in crystalline product.
(2) Matter Transfer utilization in production process, greatly saved the consumption of the raw materials such as soda ash, water, and effluxed without waste water, waste gas, environmentally friendly.
(3) the precipitated silica purity made is high, and even particle size distribution can be used as high-quality production marketing.
The accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
In figure, each strand of material means respectively:
L1: the mixture of quartz sand and soda ash;
S2-1: the water glass solid that calcining obtains;
G2-2: the CO that calcining discharges
2gas;
L3: sodium silicate solution;
L4: the suspension after crystallization reaction;
S5: hydrated SiO 2 solid;
L6-1: enter CO
2the Na of absorption section
2cO
3solution;
L6-2: enter the Na that dissolves workshop section
2cO
3solution;
L6-3: the Na that enters evaporation concentration workshop section
2cO
3solution;
L7:NaHCO
3solution;
L8: the Na after concentrated
2cO
3solution.
The SEM figure of the precipitated silica product that Fig. 2 is the embodiment of the present invention 1 preparation;
The EDS of the precipitated silica product that Fig. 3 is the embodiment of the present invention 1 preparation can spectrogram.
Embodiment
Introduce in detail the present invention below in conjunction with drawings and the specific embodiments.But following embodiment only limits to explain the present invention, protection scope of the present invention should comprise the full content of claim, is not limited only to the present embodiment.
As shown in Figure 1, at first the present invention is that to take quartz sand and soda ash be raw material, mix rear calcining and prepare water glass, again water glass is reacted with sodium hydrogen carbonate solution, by controlling the degree of supersaturation of solution, crystallization hydrated SiO 2 precipitation, the precipitation after filtration obtains precipitated silica product, the recycle of filtrate sodium carbonate through washing, drying and other steps.
600g quartz sand is mixed with 1270g soda ash, and under 1300 ℃, calcining 60min obtains solid-state water glass 1205g, reclaims CO simultaneously
2.Solid-state water glass is dissolved in sodium carbonate solution, obtains the sodium silicate solution of 1.2mol/L.
The 500mL sodium silicate solution is placed in to the crystallization reactor of 10L, temperature is controlled at 40 ℃, turn on agitator, drip with peristaltic pump the sodium hydrogen carbonate solution that concentration is 2.7mol/L, control degree of supersaturation by drop rate and the dripping quantity of adjusting solution, drip sodium hydrogen carbonate solution total amount 700mL, separate out the hydrated SiO 2 precipitation.
Suspension in the crystallization reaction still is filtered.Filtration obtains the 1160mL sodium carbonate solution, and wherein the 500mL sodium carbonate solution absorbs CO
2gas, obtain the sodium hydrogen carbonate solution of 2.7mol/L, turns back to peristaltic pump and recycle; The 300mL sodium carbonate solution is for dissolving solid-state water glass; All the other sodium carbonate solutions, through evaporation concentration, turn back to calcination process.Precipitation after filtration makes 582g precipitated silica product through washing, drying, pulverizing, and its dioxide-containing silica is 99.90wt%.
1000g quartz sand is mixed with 2650g soda ash, and under 1350 ℃, calcining 60min obtains solid-state water glass 1880g, reclaims CO simultaneously
2.Solid-state water glass is dissolved in sodium carbonate solution, obtains the sodium silicate solution of 1.2mol/L.
The 800mL sodium silicate solution is placed in to the crystallization reactor of 10L, temperature is controlled at 45 ℃, turn on agitator, drip with peristaltic pump the sodium hydrogen carbonate solution that concentration is 2.7mol/L, control degree of supersaturation by drop rate and the dripping quantity of adjusting solution, drip sodium hydrogen carbonate solution total amount 1120mL, separate out the hydrated SiO 2 precipitation.
Suspension in the crystallization reaction still is filtered.Filtration obtains the 1870mL sodium carbonate solution, and wherein the 800mL sodium carbonate solution absorbs CO
2gas, obtain the sodium hydrogen carbonate solution of 2.7mol/L, turns back to peristaltic pump and recycle; The 500mL sodium carbonate solution is for dissolving solid-state water glass; All the other sodium carbonate solutions, through evaporation concentration, turn back to calcination process.Precipitation after filtration makes 915g precipitated silica product through washing, drying, pulverizing, and its dioxide-containing silica is 99.92wt%.
Embodiment 3
1000g quartz sand is mixed with 3000g soda ash, and under 1400 ℃, calcining 60min obtains solid-state water glass 1975g, reclaims CO simultaneously
2.Solid-state water glass is dissolved in sodium carbonate solution, obtains the sodium silicate solution of 1.2mol/L.
The 1000mL sodium silicate solution is placed in to the crystallization reactor of 10L, temperature is controlled at 50 ℃, turn on agitator, drip with peristaltic pump the sodium hydrogen carbonate solution that concentration is 2.7mol/L, control degree of supersaturation by drop rate and the dripping quantity of adjusting solution, drip sodium hydrogen carbonate solution total amount 1400mL, separate out the hydrated SiO 2 precipitation.
Suspension in the crystallization reaction still is filtered.Filtration obtains the 2275mL sodium carbonate solution, and wherein the 1000mL sodium carbonate solution absorbs CO
2gas, obtain the sodium hydrogen carbonate solution of 2.7mol/L, turns back to peristaltic pump and recycle; The 600mL sodium carbonate solution is for dissolving solid-state water glass; All the other sodium carbonate solutions, through evaporation concentration, turn back to calcination process.Precipitation after filtration makes the high-purity precipitated silica product of 952g through washing, drying, pulverizing, and its dioxide-containing silica is 99.95wt%.
In a word, the precipitated silica product purity that the present invention obtains is high more than 99.9%, even particle size distribution, and whole Production Flow Chart Matter Transfer utilizes, and overcome the problem of sodium sulfate sewage discharge in conventional production.
It should be noted that, according to the various embodiments described above of the present invention, those skilled in the art are the four corners that can realize independent claim of the present invention and appurtenance fully, implementation procedure and method same the various embodiments described above; And non-elaborated part of the present invention belongs to techniques well known.
The above; be only part embodiment of the present invention, but protection scope of the present invention is not limited to this, in the technical scope that any those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.
Claims (6)
1. one kind is utilized sodium bicarbonate to control the method that degree of supersaturation is produced precipitated silica, it is characterized in that performing step is as follows:
(1) quartz sand and soda ash are prepared burden on request, calcine 30～60min and obtain solid-state water glass under 1300～1400 ℃, reclaim CO simultaneously
2; Mole proportioning of described quartz sand and soda ash is 1:(1.2～1.8);
(2) solid-state water glass dissolves in sodium carbonate solution, obtains sodium silicate solution;
(3) the resulting sodium silicate solution of step (2) is placed in to crystallization reactor, controls temperature, turn on agitator, drip sodium hydrogen carbonate solution with peristaltic pump, control degree of supersaturation by drop rate and the dripping quantity of adjusting solution, separate out the hydrated SiO 2 precipitation, obtain suspension;
(4) the resulting suspension of step (3) is filtered, obtain hydrated SiO 2 precipitation and sodium carbonate filtrate, the precipitation after filtration makes the precipitated silica product through washing, drying, pulverizing;
(5) the filtrate sodium bicarbonate that step (4) obtains divides three partially recycled utilizations: the CO that a part of sodium carbonate solution absorption step (1) obtains
2gas, control gas flow, obtains sodium hydrogen carbonate solution, turns back to step (3) and recycle; Part sodium carbonate solution turns back to step (2), for dissolving solid-state water glass; The last part sodium carbonate solution, through evaporation concentration, turns back to step (1) and is calcined.
2. method according to claim 1, it is characterized in that: the specification of the described quartz sand of step (1) is 40～70 orders, SiO
2content is 98.8%.
3. method according to claim 1, it is characterized in that: the concentration of the resulting sodium silicate solution of step (2) is 1.2mol/L.
4. method according to claim 1 is characterized in that: in step (3), the crystallization reaction actuator temperature is controlled at 40～50 ℃.
5. method according to claim 1, it is characterized in that: the concentration of the sodium hydrogen carbonate solution dripped in step (3) is 2.7mol/L.
6. method according to claim 1, it is characterized in that: described step (5) precipitated silica product purity is up to more than 99.9%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828831A (en) * | 2015-06-05 | 2015-08-12 | 确成硅化学股份有限公司 | Method for continuously producing white carbon black |
| CN105858668A (en) * | 2016-03-30 | 2016-08-17 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN107162009A (en) * | 2017-06-15 | 2017-09-15 | 确成硅化学股份有限公司 | A kind of preparation method of high structure high abrasion hydrated SiO 2 |
| CN107265466A (en) * | 2017-06-15 | 2017-10-20 | 确成硅化学股份有限公司 | A kind of fast preparation method for extruding high dispersive hydrated SiO 2 |
| CN109577076A (en) * | 2018-12-26 | 2019-04-05 | 江苏理文造纸有限公司 | A kind of filler and preparation method thereof for liner board |
| CN111620348A (en) * | 2020-06-22 | 2020-09-04 | 安徽龙泉硅材料有限公司 | Preparation method of sodium silicate for nano silicon dioxide |
| CN111777074A (en) * | 2020-06-15 | 2020-10-16 | 冷水江三A新材料科技有限公司 | Preparation method of silicon dioxide for calcium ion efficient adsorbent |
| CN112707428A (en) * | 2021-01-27 | 2021-04-27 | 北京化工大学 | Combined preparation method of nano calcium carbonate and pseudo-boehmite or white carbon black |
| CN113307279A (en) * | 2021-05-14 | 2021-08-27 | 珠海宏嘉投资有限公司 | Production method of food-grade silicon powder |
| CN115196644A (en) * | 2022-08-04 | 2022-10-18 | 安徽进化硅纳米材料科技有限公司 | Preparation method and application of silicon dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828831A (en) * | 2015-06-05 | 2015-08-12 | 确成硅化学股份有限公司 | Method for continuously producing white carbon black |
| CN105858668A (en) * | 2016-03-30 | 2016-08-17 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN105858668B (en) * | 2016-03-30 | 2017-03-22 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
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| CN109577076A (en) * | 2018-12-26 | 2019-04-05 | 江苏理文造纸有限公司 | A kind of filler and preparation method thereof for liner board |
| CN111777074A (en) * | 2020-06-15 | 2020-10-16 | 冷水江三A新材料科技有限公司 | Preparation method of silicon dioxide for calcium ion efficient adsorbent |
| CN111620348A (en) * | 2020-06-22 | 2020-09-04 | 安徽龙泉硅材料有限公司 | Preparation method of sodium silicate for nano silicon dioxide |
| CN111620348B (en) * | 2020-06-22 | 2022-11-22 | 安徽龙泉硅材料有限公司 | Preparation method of sodium silicate for nano silicon dioxide |
| CN112707428A (en) * | 2021-01-27 | 2021-04-27 | 北京化工大学 | Combined preparation method of nano calcium carbonate and pseudo-boehmite or white carbon black |
| CN113307279A (en) * | 2021-05-14 | 2021-08-27 | 珠海宏嘉投资有限公司 | Production method of food-grade silicon powder |
| CN115196644A (en) * | 2022-08-04 | 2022-10-18 | 安徽进化硅纳米材料科技有限公司 | Preparation method and application of silicon dioxide |
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