CN101323453A - Circulation novel process for preparing white carbon black - Google Patents
Circulation novel process for preparing white carbon black Download PDFInfo
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- CN101323453A CN101323453A CNA2008100482954A CN200810048295A CN101323453A CN 101323453 A CN101323453 A CN 101323453A CN A2008100482954 A CNA2008100482954 A CN A2008100482954A CN 200810048295 A CN200810048295 A CN 200810048295A CN 101323453 A CN101323453 A CN 101323453A
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- carbon black
- white carbon
- water glass
- glass solution
- mother liquor
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Abstract
The invention relates to a new cycle technique for preparing white carbon black, comprising the following steps: 1) a water glass solution reacts with an ammonium hydrogen carbonate solution or solid ammonium hydrogen carbonate in the condition of the temperature of 30 to 50 DEG C, the white carbon black is obtained and ammonia escapes simultaneously; 2) the ammonia escaped from the step 1) is mixed with CO2 gas produced in the process of the preparation of the water glass solution and the obtained mixture is absorbed by water to obtain the ammonium hydrogen carbonate; 3) the white carbon black produced by reaction is filtered under the condition of vacuum to obtain a mother liquid A and a filter cake A, the mother liquid A is recovered and the filter cake A is washed, dried and crushed so as to obtain the white carbon black. The invention 1) solves the effective recovery of by-products in the production process, is used for self-production, improves the utilization value of materials, without three wastes discharge in the production process, and has high material utilization rate, good effect of discharge reduction and stable and reliable quality of products; 2) recovery of sodium bicarbonate is carried out after the mass concentration is increased by the evaporation in vacuum at low temperature, thus reducing the usage of organic solvent.
Description
Technical field
Of the present inventionly relate to a kind of circulation novel process for preparing white carbon black.
Background technology
White carbon black is a kind of broad-spectrum inorganic fine chemical product; traditional production method is to adopt the precipitator method; with water glass is raw material; carry out replacement(metathesis)reaction with sulfuric acid or hydrochloric acid and make; can produce sodium sulfate or the sodium chloride aqueous solution that concentration is low, liquid measure is big in this technological process, reclaim the low material of this class concentration, consume a large amount of energy; the outwards discharging as not recycled is certain to environment is caused severe contamination or is unfavorable for the protection of ecotope.This traditional production method is all to have great technological deficiency to enterprise or to country and society.
Summary of the invention
Problem to be solved by this invention is to propose a kind of circulation novel process for preparing white carbon black at above-mentioned prior art, this technology can save energy consumption, reduce to produce the pollution that waste causes environment and water body, reduce production costs basic demands such as realization is energy-saving and cost-reducing, reduction of discharging to a great extent.
The present invention for the solution that problem adopts of the above-mentioned proposition of solution is: a kind of circulation novel process for preparing white carbon black includes following steps:
1) makes water glass solution by existing technology, under 30-50 ℃ of condition with the water glass solution of 9-10 ° of Be ' with ammonium bicarbonate soln or solid ammonium bicarbonate with and add mode carry out stirring reaction, water glass solution and bicarbonate of ammonia mole proportioning are 1: 2.0～1: 2.2, the throw out white carbon black that obtains loosening, the ammonia of overflowing simultaneously;
2) with above-mentioned steps 1) ammonia of overflowing is with the CO that produces in the water glass solution preparation process
2Gas is mixed together and water absorbs, and makes the bicarbonate of ammonia that is used for carrying out with water glass solution replacement(metathesis)reaction;
3) the throw out white carbon black that the step 1) reaction is made filters under vacuum condition, obtains mother liquor first and filter cake first, and the mother liquor first reclaims, and the filter cake first promptly obtains the white carbon black of polymolecularity through washing, drying, pulverizing.
Press such scheme, it is to filter in the mother liquor first that obtains to contain the sodium bicarbonate that mass concentration is 10%-12% under vacuum condition that step 3) mother liquor first reclaims, being evaporated to mass concentration through vacuum and low temperature is 25%-30%, reduce to room temperature, add organic solvent, stirring and evenly mixing can therefrom be separated out a large amount of NaHCO
3Crystal filters, and obtains mother liquor second and filter cake second, and filter cake second is carried out pyroreaction after mixing with quartz mine in molar ratio 2: 3.1-3.4 after drying in horseshoe flame furnace, make solid water glass; Mother liquor second then in distillation tower with low-pressure steam heating, under 78-80 ℃ of temperature condition, reclaim and obtain organic solvent, the hot water that steams after surplus then is used for dissolved solids water glass and makes water glass solution.
Press such scheme, described low-pressure steam is to adopt recovery waste heat in the water glass solution preparation process and the low-pressure steam that produces.
Press such scheme, described organic solvent is dehydrated alcohol, anhydrous methanol or anhydrous propyl alcohol.
The main raw material of whole process of preparation is natural crystal-quartz sand, and all the other raw materials then recycle in system, suitably adds because the loss part that evaporating, emitting, dripping or leaking of liquid or gas caused.Principal reaction equation of the present invention is Na
2OmSiO
2+ 2NH
4HCO
3→ 2NaHCO
3+ mSiO
2NH
2O ↓+2NH
3The H of ↑+(1-mn)
2O.
Advantage of the present invention:
1) the present invention has reasonably solved the efficient recovery of by product in the production process, and is used for self production, has improved the starting material recycle greatly and has been worth, and promptly the sodium bicarbonate of Hui Shouing is used to prepare water glass, and the ammonia of effusion contains CO with calcining workshop section
2The high temperature kiln after the waste heat boiler recovery waste heat produces low-pressure steam, enter absorption unit together, water absorbs makes ammonium bicarbonate aqueous solution, organic solvent is through also recycling in system after the underpressure distillation, the surplus water of heat then is used to dissolve water glass, make and accomplish three-waste free discharge in the whole process of production, the utilization rate of raw materials height, its emission reduction effect is good, the white carbon black production cost can reduce more than 50%, stable and reliable product quality.
2) sodium bicarbonate in the mother liquor first is reclaimed after the vacuum and low temperature evaporation raises mass concentration again, significantly reduced the usage quantity of organic solvent.
Description of drawings
Fig. 1 is the circulation technology schematic flow sheet that the present invention prepares white carbon black.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
As Fig. 1, be that 3.2 water glass is configured to 10 ° of Be ' after purifying treatment dilute solution 300ml joins in the stirred reactor of 1000ml with modulus, keep reaction mass 45 ℃ of scopes, add 20g while stirring through purified NH
4HCO
3, make it to carry out following reaction: Na
2OmSiO
2+ 2NH
4HCO
3=2NaHCO
3+ mSiO
2NH
2O ↓+2NH
3The H of ↑+(1-mn)
2O, wherein water glass solution and NH
4HCO
3Mol ratio be controlled at 1: 2.0～1: 2.2 (wherein 3.1＜m＜3.4), behind the reaction 45-60min, can't smell ammonia flavor (available moistening test paper is checked it) then for reaction finishes from the reactor head evolving gas, the throw out white carbon black that obtains loosening.
The throw out that above-mentioned reaction is made filters under vacuum condition, obtain filter cake first and mother liquor first, initial mother liquor first is removed 1/3 moisture through vacuum and low temperature evaporation after, making the mass concentration of sodium bicarbonate in the mother liquor first is 25%-30%, be cooled to room temperature, add the 150ml dehydrated alcohol, and carry out vigorous stirring, leave standstill 5min, separate out NaHCO
3Crystal, after filtration, drying obtains NaHCO
3Be 20.81g, reclaiming transformation efficiency is 97.88%, and obtains mother liquor second; Mother liquor second then heats with low-pressure steam in distillation tower, carries out vacuum distilling under 80 ℃ of conditions, reclaims dehydrated alcohol 145.1ml, and the rate of recovery is 96.7%.NaHCO
3Then by existing routine techniques prepared water glass solution.
The filter cake first is washed till pH=6.5～7.5 scopes through ultrasonic wave, dewaters, dry 2h under 120 ℃ pulverizes 5min through Universalpulverizer, obtains the white carbon black 14.37g of ultrafine powder powder, and ult rec reached for 95% (various losses add up to 5%).
Embodiment 2
As Fig. 1, be that 3.2 water glass is configured to 9 ° of Be ' after purifying treatment dilute solution 300ml joins in the stirred reactor of 1000ml with modulus, keep reaction mass 30 ℃ of scopes, add 19g while stirring through purified NH
4HCO
3, make it to carry out following reaction: Na
2OmSiO
2+ 2NH
4HCO
3=2NaHCO
3+ mSiO
2NH
2O ↓+2NH
3The H of ↑+(1-mn)
2O, wherein water glass solution and NH
4HCO
3Mol ratio be controlled at 1: 2.0～1: 2.2 (wherein 3.1＜m＜3.4), behind the reaction 45-60min, can't smell ammonia flavor (available moistening test paper is checked it) then for reaction finishes from the reactor head evolving gas, the throw out white carbon black that obtains loosening.
The throw out that above-mentioned reaction is made filters under vacuum condition, obtain filter cake first and mother liquor first, initial mother liquor first is removed 1/3 moisture through vacuum and low temperature evaporation after, making the mass concentration of sodium bicarbonate in the mother liquor first is 25%-30%, be cooled to room temperature, add the 150ml anhydrous methanol, and carry out vigorous stirring, leave standstill 5min, separate out NaHCO
3Crystal, after filtration, drying obtains NaHCO
3Be 19.76g, reclaiming transformation efficiency is 97.56%, and obtains mother liquor second; Mother liquor second then heats with low-pressure steam in distillation tower, carries out vacuum distilling under 78 ℃ of conditions, reclaims anhydrous methanol 145.5ml, and the rate of recovery is 96.30%.NaHCO
3Then by existing routine techniques prepared water glass solution.
The filter cake first is washed till pH=6.5～7.5 scopes through ultrasonic wave, dewaters, dry 2h under 120 ℃ pulverizes 5min through Universalpulverizer, obtains the white carbon black 13.86g of ultrafine powder powder, and ult rec reached for 95.46% (various losses add up to 4.54%).
Claims (4)
1, a kind of circulation novel process for preparing white carbon black is characterized in that including following steps:
1) makes water glass solution by existing technology, under 30-50 ℃ of condition with the water glass solution of 9-10 ° of Be ' with ammonium bicarbonate soln or solid ammonium bicarbonate with and add mode carry out stirring reaction, water glass solution and bicarbonate of ammonia mole proportioning are 1: 2.0～1: 2.2, the throw out white carbon black that obtains loosening, the ammonia of overflowing simultaneously;
2) with above-mentioned steps 1) ammonia of overflowing is with the CO that produces in the water glass solution preparation process
2Gas is mixed together and water absorbs, and makes the bicarbonate of ammonia that is used for carrying out with water glass solution replacement(metathesis)reaction;
3) the throw out white carbon black that the step 1) reaction is made filters under vacuum condition, obtains mother liquor first and filter cake first, and the mother liquor first reclaims, and the filter cake first promptly obtains the white carbon black of polymolecularity through washing, drying, pulverizing.
2, by the described a kind of circulation novel process for preparing white carbon black of claim 1, it is characterized in that it is to filter in the mother liquor first that obtains to contain the sodium bicarbonate that mass concentration is 10%-12% that step 3) mother liquor first reclaims under vacuum condition, being evaporated to mass concentration through vacuum and low temperature is 25%-30%, reduce to room temperature, add organic solvent, stirring and evenly mixing can therefrom be separated out a large amount of NaHCO
3Crystal filters, and obtains mother liquor second and filter cake second, and filter cake second is carried out pyroreaction after mixing with quartz mine in molar ratio 2: 3.1-3.4 after drying in horseshoe flame furnace, make solid water glass; Mother liquor second then in distillation tower with low-pressure steam heating, under 78-80 ℃ of temperature condition, reclaim and obtain organic solvent, the hot water that steams after surplus then is used for dissolved solids water glass and makes water glass solution.
3,, it is characterized in that described low-pressure steam is to adopt recovery waste heat in the water glass solution preparation process and the low-pressure steam that produces by the described a kind of circulation novel process for preparing white carbon black of claim 2.
4,, it is characterized in that described organic solvent is dehydrated alcohol, anhydrous methanol or anhydrous propyl alcohol by claim 2 or 3 described a kind of circulation novel process that prepare white carbon black.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100482954A CN101323453B (en) | 2008-07-04 | 2008-07-04 | Circulation novel process for preparing white carbon black |
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|---|---|---|---|
| CN2008100482954A CN101323453B (en) | 2008-07-04 | 2008-07-04 | Circulation novel process for preparing white carbon black |
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| CN101323453A true CN101323453A (en) | 2008-12-17 |
| CN101323453B CN101323453B (en) | 2012-05-23 |
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ID=40187184
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092723A (en) * | 2011-03-30 | 2011-06-15 | 廖险峰 | Method for preparing high dispersing white carbon black with ammonia precipitation method |
| CN102633272A (en) * | 2012-04-19 | 2012-08-15 | 浙江宇达化工有限公司 | Preparation method of precipitated silicon dioxide |
| CN102633266A (en) * | 2012-04-19 | 2012-08-15 | 浙江宇达化工有限公司 | Preparation method of nano SiO2 |
| CN102765724A (en) * | 2012-04-19 | 2012-11-07 | 浙江宇达化工有限公司 | Preparation method of silica gel |
| CN103601217A (en) * | 2013-11-26 | 2014-02-26 | 于岩 | Sodium fluoride production process and sodium fluoride mother liquor recycling process |
| CN103638834A (en) * | 2013-12-17 | 2014-03-19 | 青岛东岳泡花碱有限公司 | Method for dissolving sodium silicate by virtue of static pressure kettle |
| 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 |
| CN109956481A (en) * | 2019-04-02 | 2019-07-02 | 原初科技（北京）有限公司 | The method for preparing ammonia using ammonium salt and silicate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1005407B (en) * | 1986-09-15 | 1989-10-11 | 华东化工学院 | Prodn. of bicarbonate of ammonium by method of ammonium/carbon balance |
| CN1037110C (en) * | 1993-06-18 | 1998-01-21 | 鞍山钢铁学院 | Method for producing silica white |
-
2008
- 2008-07-04 CN CN2008100482954A patent/CN101323453B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092723A (en) * | 2011-03-30 | 2011-06-15 | 廖险峰 | Method for preparing high dispersing white carbon black with ammonia precipitation method |
| CN102633272A (en) * | 2012-04-19 | 2012-08-15 | 浙江宇达化工有限公司 | Preparation method of precipitated silicon dioxide |
| CN102633266A (en) * | 2012-04-19 | 2012-08-15 | 浙江宇达化工有限公司 | Preparation method of nano SiO2 |
| CN102765724A (en) * | 2012-04-19 | 2012-11-07 | 浙江宇达化工有限公司 | Preparation method of silica gel |
| WO2013155975A1 (en) * | 2012-04-19 | 2013-10-24 | 浙江宇达化工有限公司 | Preparation method for precipitated silica |
| CN103601217A (en) * | 2013-11-26 | 2014-02-26 | 于岩 | Sodium fluoride production process and sodium fluoride mother liquor recycling process |
| CN103638834A (en) * | 2013-12-17 | 2014-03-19 | 青岛东岳泡花碱有限公司 | Method for dissolving sodium silicate by virtue of static pressure kettle |
| 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 |
| CN109956481A (en) * | 2019-04-02 | 2019-07-02 | 原初科技（北京）有限公司 | The method for preparing ammonia using ammonium salt and silicate |
| CN109956481B (en) * | 2019-04-02 | 2020-03-10 | 原初科技（北京）有限公司 | Method for preparing ammonia gas by using ammonium salt and silicate |
| WO2020199451A1 (en) * | 2019-04-02 | 2020-10-08 | 原初科技（北京）有限公司 | Method for preparing ammonia by using ammonium salt and silicate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101323453B (en) | 2012-05-23 |
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