CN102432025A - Production method for precipitated silica - Google Patents

Production method for precipitated silica Download PDF

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Publication number
CN102432025A
CN102432025A CN2011102752606A CN201110275260A CN102432025A CN 102432025 A CN102432025 A CN 102432025A CN 2011102752606 A CN2011102752606 A CN 2011102752606A CN 201110275260 A CN201110275260 A CN 201110275260A CN 102432025 A CN102432025 A CN 102432025A
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CN
China
Prior art keywords
drying
silicic acid
precipitated silica
temperature
ammonium chloride
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Pending
Application number
CN2011102752606A
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Chinese (zh)
Inventor
田伟
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CHIPING COUNTY XINFA SHENGJI RED MUD TREATMENT Co Ltd
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CHIPING COUNTY XINFA SHENGJI RED MUD TREATMENT Co Ltd
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Priority to CN2011102752606A priority Critical patent/CN102432025A/en
Publication of CN102432025A publication Critical patent/CN102432025A/en
Pending legal-status Critical Current

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Abstract

The invention provides a production method for precipitated silica. The method comprises the following steps: firstly, adding acid-containing silicic acid gel and ammonia water with a concentration of 18% according to a weight ratio of 0.8-1.0:0.30-0.34 into a reaction pot for pulping and adding water which accounts for 20 to 25% of the mass of the silicic acid gel for stirring; secondly, pumping obtained slurry into a chamber filter press with a stainless steel pump for solid-liquid separation, with temperature for press filtration being normal temperature and pressure being 0.6 to 0.8 MPa; finally, rinsing solid obtained in the previous step with water twice, wherein, 15 tons of water is used for rinsing each ton of silicic acid gel, and delivering a material obtained after rinsing into a flash dryer for crushing and drying so as to obtain a finished product of precipitated silica, wherein, temperature for drying is 300 to 350 DEG C, time for drying is 20 to 30 min, obtained liquid is rich in the component of ammonium chloride, ammonium chloride with a high purity of 90 to 98% can be obtained by condensing and drying the liquid, and rest rinsing water is returned to a production line for cyclic utilization after deposition and regeneration. The method has the characteristics of a simple process, safety, reliability, low energy consumption, great treating capacity, no pollution, small investment, stable and excellent product quality and low cost.

Description

A kind of working method of precipitated silica
Technical field
The invention belongs to the silicon compound production technical field, be specifically related to a kind of working method of precipitated silica.
Background technology
The production technique of existing precipitated silica is to adopt fuel oil or fat coal at high temperature silica sand and soda ash reaction to be made service water glass, and service water glass water is mixed with certain density dilute solution.Add certain acid then under certain condition, precipitation of silica is come out, through cleaning, filtration, dry (oven dry or spraying) are pulverized and are made precipitated silica again.Its shortcoming is: need fire water glass, also will add acid and ageing and handle, so complex manufacturing.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art; The object of the present invention is to provide a kind of working method of precipitated silica; It is simple to have technology, safe and reliable, energy consumption is low, treatment capacity is big, pollution-free, investment is little, constant product quality is good and with low cost characteristics.
To achieve these goals, the technical scheme of the present invention's employing is: a kind of working method of precipitated silica may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 0.8~1.0: 0.30~0.34 ratio adds the making beating of neutralization reaction jar with weight ratio, and adds water in the ratio of silicic acid gel quality 20-25% and stir, and adjustment slurry pH value is to 6-8;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.6-0.8mpa;
At last, will go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton; Material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 300-350 ℃, and be 20-30min time of drying, and gained liquid is rich in the ammonium chloride composition; Behind concentrate drying, can make high-purity ammonium chloride of 90~98%, return the production line recycle after all the other washing water by precipitation regeneration.
Because the present invention utilizes relieving haperacidity co-production WHITE CARBON BLACK; And be non-airtight; Carry out under non high temperature, the condition of high voltage, adopt in the first-level alkali adding (ammoniacal liquor) to add the water washing measure, can make purity and be high-purity ammonium chloride of 90~98% with secondary; It is simple to have technology, safe and reliable, energy consumption is low, treatment capacity is big, pollution-free, investment is little, constant product quality is good and with low cost characteristics.
Embodiment
Below in conjunction with embodiment the present invention is done further explain.
Embodiment one
A kind of working method of precipitated silica may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 1.0: 0.32 ratio adds the making beating of neutralization reaction jar with mass ratio, and adds water in the ratio of silicic acid gel quality 20% and stir,, the pH value to 6 of adjustment slurry;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.6mpa;
At last, will go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton; Material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 300 ℃, and be 30min time of drying, and gained liquid is rich in the ammonium chloride composition; Behind concentrate drying, can make high-purity ammonium chloride of 90%, return the production line recycle after all the other washing water by precipitation regeneration.
Because the present invention utilizes relieving haperacidity co-production WHITE CARBON BLACK; And be non-airtight; Carry out under non high temperature, the condition of high voltage, adopt in the first-level alkali adding (ammoniacal liquor) to add the water washing measure with secondary, the purity that can make is high-purity ammonium chloride of 90%; It is simple to have technology, safe and reliable, energy consumption is low, treatment capacity is big, pollution-free, investment is little, constant product quality is good and with low cost characteristics.
Embodiment two
A kind of working method of precipitated silica may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 0.8: 0.30 ratio adds the making beating of neutralization reaction jar with weight ratio, and adds water in the ratio of silicic acid gel quality 25% and stir,, the pH value to 8 of adjustment slurry;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.8mpa;
At last, will go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton; Material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 350 ℃, and be 20min time of drying, and gained liquid is rich in the ammonium chloride composition; Behind concentrate drying, can make high-purity ammonium chloride of 95%, return the production line recycle after all the other washing water by precipitation regeneration.
Because the present invention utilizes relieving haperacidity co-production WHITE CARBON BLACK, and is non-airtight, carry out under non high temperature, the condition of high voltage, adopt in the first-level alkali adding (ammoniacal liquor) to add the water washing measure with secondary, the purity that can make is high-purity ammonium chloride of 95%.
Embodiment three
A kind of working method of precipitated silica may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 0.9: 0.34 ratio adds the making beating of neutralization reaction jar with weight ratio, and adds water in the ratio of silicic acid gel quality 23% and stir the pH value to 7 of adjustment slurry;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.7mpa;
At last, will go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton; Material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 330 ℃, and be 25min time of drying, and gained liquid is rich in the ammonium chloride composition; Behind concentrate drying, can make high-purity ammonium chloride of 98%, return the production line recycle after all the other washing water by precipitation regeneration.
Because the present invention utilizes relieving haperacidity co-production WHITE CARBON BLACK, and is non-airtight, carry out under non high temperature, the condition of high voltage, adopt in the first-level alkali adding (ammoniacal liquor) to add the water washing measure with secondary, the purity that can make is high-purity ammonium chloride of 98%.

Claims (4)

1. the working method of a precipitated silica is characterized in that, may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 0.8~1.0: 0.30~0.34 ratio adds the making beating of neutralization reaction jar with mass ratio, and adds water in the ratio of silicic acid gel quality 20-25% and stir, and adjustment slurry pH value is to 6-8;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.6-0.8mpa;
At last; To go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton, and the material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 300-350 ℃; Be 20-30min time of drying, and gained liquid is rich in the ammonium chloride composition, behind concentrate drying, can make high-purity ammonium chloride of 90~98%.
2. the working method of a kind of precipitated silica according to claim 1 is characterized in that, may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 1.0: 0.32 ratio adds the making beating of neutralization reaction jar with weight ratio, and adds water in the ratio of silicic acid gel quality 20% and stir,, the pH value to 6 of adjustment fetters;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.6-0.8mpa;
At last; To go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton, and the material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 300 ℃; Be 30min time of drying, and gained liquid is rich in the ammonium chloride composition, through making the high-purity ammonium chloride more than 90% behind the concentrate drying.
3. the working method of a kind of precipitated silica according to claim 1 is characterized in that, may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 0.8: 0.30 ratio adds the making beating of neutralization reaction jar with weight ratio, and adds water in the ratio of silicic acid gel quality 25% and stir,, the pH value to 8 of adjustment fetters;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.8mpa;
At last; To go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton, and the material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 350 ℃; Be 20min time of drying, and gained liquid is rich in the ammonium chloride composition, behind concentrate drying, can make high-purity ammonium chloride of 95%.
4. the working method of a kind of precipitated silica according to claim 1 is characterized in that, may further comprise the steps:
At first, the ammoniacal liquor that will contain sour silicic acid gel and 18% is that 0.9: 0.34 ratio adds the making beating of neutralization reaction jar with weight ratio, and adds water in the ratio of silicic acid gel quality 23% and stir the pH value to 7 of adjustment fetters;
Secondly, above-mentioned slurry is sent into chamber(filter)press with Stainless Steel Pump carry out solid-liquid separation, the temperature of press filtration is a normal temperature, and pressure is 0.7mpa;
At last; To go up step gained solid and carry out adding water washing twice, the bath water amount is 15 tons of silicic acid gels per ton, and the material after the washing is sent into and is the precipitated silica finished product after flash dryer is pulverized drying; Drying temperature is 330 ℃; Be 25min time of drying, and gained liquid is rich in the ammonium chloride composition, behind concentrate drying, can make high-purity ammonium chloride of 98%.
CN2011102752606A 2011-09-16 2011-09-16 Production method for precipitated silica Pending CN102432025A (en)

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CN2011102752606A CN102432025A (en) 2011-09-16 2011-09-16 Production method for precipitated silica

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Application Number Priority Date Filing Date Title
CN2011102752606A CN102432025A (en) 2011-09-16 2011-09-16 Production method for precipitated silica

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CN102432025A true CN102432025A (en) 2012-05-02

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407324A (en) * 2008-06-02 2009-04-15 通化双龙化工股份有限公司 Method of preparing silicon dioxide delustrant by large pore volume gel
CN102180472A (en) * 2010-12-19 2011-09-14 何侠 Method for preparing water glass and activated silica gel by using waste residues from treatment of sulfuric acid cinder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407324A (en) * 2008-06-02 2009-04-15 通化双龙化工股份有限公司 Method of preparing silicon dioxide delustrant by large pore volume gel
CN102180472A (en) * 2010-12-19 2011-09-14 何侠 Method for preparing water glass and activated silica gel by using waste residues from treatment of sulfuric acid cinder

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Application publication date: 20120502