CN105712361A - Production method of food additive white carbon black - Google Patents
Production method of food additive white carbon black Download PDFInfo
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- CN105712361A CN105712361A CN201610170860.9A CN201610170860A CN105712361A CN 105712361 A CN105712361 A CN 105712361A CN 201610170860 A CN201610170860 A CN 201610170860A CN 105712361 A CN105712361 A CN 105712361A
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- white carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a production method of an inorganic powder material, in particular to a production method of food additive white carbon black. White carbon black precipitates for a synthetic reaction, wherein a certain quantity of prepared sodium silicate solution is put into a reaction kettle and serves as a backing material, then 5 m<3> of water is added, vapor is introduced, stirring starts when temperature is raised to 50-55 DEG C, temperature continues to be raised to 86-88 DEG C, reaction time is 40 min, and a pH value is controlled between 9 and 11; secondly, sodium silicate and dilute sulphuric acid are added into the reaction kettle according to the flow for synthesis reaction, reaction time is 50 min, reaction temperature is 86-88 DEG C, and a pH value is controlled between 10 and 11 during reaction; thirdly, dilute sulphuric acid continues to be added, a terminal point pH value is adjusted to be 4-5, stirring continues, and after aging is performed for 30 min, stirring stops. By optimizing technological parameters, the requirements of improving the porosity and enhancing the adsorption performance are met, and the defects that in a common precipitation method, the porosity of white carbon black is low, and the adsorption performance is poor are overcome.
Description
Technical field
The present invention relates to the production method of a kind of inorganic powder material, be specifically related to be applied to the production method of a kind of food additive white carbon.
Background technology
In the prior art, the fields such as precipitated silica is a kind of widely used inorganic functional powder body material, is mainly used in General Purpose Rubber, silicone rubber, coating, ink, pesticide, papermaking, food additive.Be mainly the sedimentation method for food additive white carbon black production method, its shortcoming be raw material be not food stage, ordinary precipitation process white carbon porosity is low, adsorptivity difference and the shortcoming in food can not be added to.
Summary of the invention
It is an object of the present invention to provide the production method of a kind of food additive white carbon.Solve powdery medicine (food) and store long-time rear easily caking, the technical problem of poor fluidity.Raw material involved in the present invention is food stage, overcomes ordinary precipitation process white carbon porosity low, and adsorptivity is poor and can not add the shortcoming in food to.
The technical scheme is that the production method of a kind of food additive white carbon, operating procedure includes the dissolving of waterglass and refines, and waterglass and dilute sulfuric acid carry out synthetic reaction, filter pressing, washing, slurrying, drying process, it is characterized in that: waterglass is carried out with dilute sulfuric acid synthetic reaction point three-step approach, first generate crystal seed, carry out synthetic reaction, the overall pH value of finally regulation again, specifically comprise the following steps that
(1) Purified Water glass solution: first carry out sodium silicate dissolving, then sodium silicate solution is configured to 1.075-1.095g/cm3, sodium oxide content is at 2.40-2.45%, and dioxide-containing silica is standby after 7.8-8.2%, plate-and-frame filtration.
(2) precipitated silica synthetic reaction: a certain amount of water glass solution prepared is squeezed in reactor, as bed material, it is subsequently adding water, it is passed through steam, is warming up to when 50-55 DEG C open stirring, is continuously heating to 86-88 DEG C, response time is 40 minutes, control ph is between 9-11, and one section of reaction puts into dilute bed material concentration after bed material, and purpose is in order to improve specific surface area of finished products.Second step, again waterglass, dilute sulfuric acid are simultaneously introduced in reactor according to flow (preferably 1:4.5 ratio), carrying out synthetic reaction, the response time is 50 minutes, reaction temperature 86-88 DEG C, reaction controlling pH value is between 10-11, this section passes through Optimizing Process Parameters, improves degree of neutralization, accelerates reaction rate, generate smaller particles, to improve porosity and the specific surface area of product.Control response time and degree of neutralization about 90%, fast-growth again on the basis of crystal seed, generate particle compared with little, specific surface area big, porosity is big, the design objective that adsorptivity is strong.3rd step, continuously adds dilute sulfuric acid, and regulation endpoint pH, at 4-5, stops stirring after continuing stirring ageing 30 minutes.Adjust product pH value, neutralize remaining water glass solution.
(3) reacting slurry after ageing is carried out filter pressing washing, in two steps:
A: the filter cake becoming solid content to be 17-20% serosity filter pressing.
B: be passed through and reach the industrial water of drinking water standard and wash, wash substantial amounts of sodium sulfate in filter cake off.
(4) slurrying: filter cake is delivered to making beating by belt conveyor and filled, and by high speed and two kinds of stir mode slurrying of low speed, provides uniform serosity for being spray-dried.
(5) drying process: the spray-dried tower of serosity is dried, then it is crushed to particle diameter less than 5 μm, after pocket type pulsed dust collector collection, packaging warehouse-in through mechanical crusher.
Step (2) bed material input amount accounts for 2/3rds of total inventory, and reaction temperature is low, dilutes bed material concentration after adding water, to increase product specific surface area, produces overall process and performs according to food additive production requirement.
In step (5), serosity inlet temperature of stabilizer is at 480-500 DEG C.
As food additive anticaking agents silicon dioxide, being dried and mobility of powdery medicine (food) can be kept, prevent caking phenomenon for a long time.
Precipitated silica production method of the present invention, with liquid soluble glass, concentrated sulphuric acid as raw material, prepares through precipitation, filter pressing, slurrying, spray drying, and product oil factor is high, porosity is big, and adsorptivity is strong, and chemical property is the most stable, nontoxic, tasteless, to inside of human body without pathologic feature after eating.
The method have the advantages that: 1, the present invention uses syllogic to react, and in the reaction by diluted material concentration, reduce reaction temperature, strictly control reaction condition, can effectively control the particle diameter of product offspring, greatly enhancing product specific surface area, product oil factor is high, and porosity is big, adsorptivity is strong, chemical property is the most stable, nontoxic, tasteless, to inside of human body without pathologic feature after eating, raw material of the present invention is easy to get, process is easily controlled, it is not necessary to increase equipment, produces overall process and performs according to food additive production requirement.
2, by tradition precipitated silica production method is improved, by Optimizing Process Parameters, reach to improve porosity, strengthen the requirement of absorption property, overcome ordinary precipitation process white carbon porosity low, the shortcoming of adsorptivity difference.3, product oil factor of the present invention is high, and specific surface area reaches more than 90% at 220-300/g, dioxide-containing silica, is dried moisture 4.5-5.5%.4, as food additive anticaking agents silicon dioxide, being dried and mobility of powdery medicine (food) can be kept, prevent caking phenomenon for a long time.
Below in conjunction with specific embodiment, the present invention is described in further details.
Detailed description of the invention
Embodiment 1
The production method concrete operation step of food additive white carbon is as follows:
1, waterglass refines
Take the waterglass that 40m dissolves through steam, be configured to the waterglass that proportion is 1.080g/ cm, through plate-and-frame filtration, take clear liquid standby.
2, the synthesis of silicon dioxide
In the reactor of 55m, add the bed material of 22m, be simultaneously introduced 5m water, be passed through steam and heat up, temperature rises to open stirring when 50 DEG C, continuing to heat up, temperature reaches to start to drip when 86 DEG C sulphuric acid, and sulphuric acid drips 0.2m per hour, react to pH value between 10-11, starting second-stage reaction, be simultaneously added dropwise waterglass and sulphuric acid, waterglass drips 11m per hour, sulphuric acid drips 0.27m per hour, and reaction is extremely
PH value stops dropping between 10-11, proceeds by three sections of reactions, drips sulphuric acid, regulates reaction end pH value, and flow is 0.38m per hour, regulates to pH value between 4.0-5.0, and synthetic reaction terminates, and is aged 30 minutes.
3, reacting slurry filter pressing, washing
Reacted serosity carries out solid, liquid separation by filter press, and the water washing using electrical conductivity to be 100us/cm is less than 1000us/cm, sodium sulphate content ＜ 0.5% to electrical conductivity.
4, slurrying
Filter cake is delivered to making beating by belt conveyor and is filled, and by high speed and two kinds of stir mode slurrying of low speed, provides uniform serosity for being spray-dried.
5, drying process
The spray-dried tower of serosity is dried, then is crushed to particle diameter less than 5 μm, after pocket type pulsed dust collector collection, packaging warehouse-in through mechanical crusher.
Embodiment 2
The production method concrete operation step of food additive white carbon is as follows:
1, waterglass refines
Take the waterglass that 50m dissolves through steam, be configured to the waterglass that proportion is 1.085g/ cm, through plate-and-frame filtration, take clear liquid standby.
2, the synthesis of silicon dioxide
The bed material of 23m is added in the reactor of 55m, it is simultaneously introduced 7m water, it is passed through steam to heat up, temperature rises to open stirring when 45 DEG C, continue to heat up, temperature reaches to start to drip sulphuric acid when 87 DEG C, sulphuric acid drips 0.21m per hour, react to pH value between 10-11, start second-stage reaction, it is simultaneously added dropwise waterglass and sulphuric acid, waterglass drips 10m per hour, sulphuric acid drips 0.19m per hour, react and stop dripping between 10-11 to pH value, proceed by three sections of reactions, dropping sulphuric acid, regulation reaction end pH value, flow is 0.35m per hour, regulate to pH value between 4.0-5.0, synthetic reaction terminates, it is aged 30 minutes.
3, reacting slurry filter pressing, washing
Reacted serosity carries out solid, liquid separation by filter press, and the water washing using electrical conductivity to be 100us/cm is less than 1000us/cm, sodium sulphate content ＜ 0.5% to electrical conductivity.
4, slurrying
Filter cake is delivered to making beating by belt conveyor and is filled, and by high speed and two kinds of stir mode slurrying of low speed, provides uniform serosity for being spray-dried.
5, drying process
The spray-dried tower of serosity is dried, then is crushed to particle diameter less than 5 μm, after pocket type pulsed dust collector collection, packaging warehouse-in through mechanical crusher.
Specific embodiment interpretation of result
The white carbon that both examples above prepares is shown in Table one with the performance indications contrast of common white white carbon black.
Table one each product aggregative indicator contrasts
| Project | Embodiment one | Embodiment two | Common white white carbon black |
| Dioxide-containing silica % | 94.82 | 94.76 | 92.36 |
| Specific surface area/g | 220 | 245 | 186 |
| Absorption value ml/g | 2.9 | 3.0 | 2.54 |
| Apparent specific gravity (gd) g/ cm3 | 0.12 | 0.08 | 0.16 |
| Particle diameter μm | 4.48 | 4.59 | 12.49 |
| PH value | 5.5 | 5.8 | 6.5 |
Can be seen that from above-mentioned two example, the present invention uses syllogic to react, and in the reaction by diluted material concentration, reduce reaction temperature, strictly control reaction condition, can effectively control the particle diameter of product offspring, greatly enhance product specific surface area, product oil factor is high, porosity is big, and adsorptivity is strong, and chemical property is the most stable, nontoxic, tasteless, being easy to get inside of human body without pathologic feature, raw material of the present invention after Shi Yong, process is easily controlled, need not increase equipment, produce overall process and perform according to food additive production requirement.
Claims (3)
1. the production method of a food additive white carbon, operating procedure includes the dissolving of waterglass and refines, and waterglass and dilute sulfuric acid carry out synthetic reaction, filter pressing, washing, slurrying, drying process, it is characterized in that: waterglass is carried out with dilute sulfuric acid synthetic reaction point three-step approach, first generate crystal seed, carry out synthetic reaction, the overall pH value of finally regulation again, specifically comprise the following steps that
(1) Purified Water glass solution: first carry out sodium silicate dissolving, then sodium silicate solution is configured to 1.075-1.095g/cm3, sodium oxide content is at 2.40-2.45%, and dioxide-containing silica is standby after 7.8-8.2%, plate-and-frame filtration；
(2) precipitated silica synthetic reaction: a certain amount of water glass solution prepared is squeezed in reactor, as bed material, it is subsequently adding water, it is passed through steam, it is warming up to when 50-55 DEG C open stirring, it is continuously heating to 86-88 DEG C, response time is 40 minutes, control ph is between 9-11, second step, again by waterglass, dilute sulfuric acid is simultaneously introduced in reactor according to flow, carry out synthetic reaction, response time is 50 minutes, reaction temperature 86-88 DEG C, reaction controlling pH value is between 10-11, 3rd step, continuously add dilute sulfuric acid, regulation endpoint pH is at 4-5, stirring is stopped after continuing stirring ageing 30 minutes；
(3) reacting slurry after ageing is carried out filter pressing washing, in two steps:
A: the filter cake becoming solid content to be 17-20% serosity filter pressing；
B: be passed through and reach the industrial water of drinking water standard and wash, wash substantial amounts of sodium sulfate in filter cake off；
(4) slurrying: filter cake is delivered to making beating by belt conveyor and filled, and by high speed and two kinds of stir mode slurrying of low speed, provides uniform serosity for being spray-dried；
(5) drying process: the spray-dried tower of serosity is dried, then it is crushed to particle diameter less than 5 μm, after pocket type pulsed dust collector collection, packaging warehouse-in through mechanical crusher.
The production method of food additive white carbon the most according to claim 1, is characterized in that: step (2) bed material input amount accounts for 2/3rds of total inventory.
The production method of food additive white carbon the most according to claim 1, is characterized in that: in step (5), serosity inlet temperature of stabilizer is at 480-500 DEG C.
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| CN201610170860.9A CN105712361A (en) | 2016-03-24 | 2016-03-24 | Production method of food additive white carbon black |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241816A (en) * | 2016-07-20 | 2016-12-21 | 福建远翔新材料股份有限公司 | A kind of preparation method of silica dioxide delustring agent |
| CN107720762A (en) * | 2017-11-29 | 2018-02-23 | 通化双龙硅材料科技有限公司 | The production method of alkaline white carbon |
| CN110150272A (en) * | 2019-06-05 | 2019-08-23 | 确成硅化学股份有限公司 | A kind of dedicated white carbon black of farm chemical carrier and preparation method thereof |
| CN110589843A (en) * | 2019-10-23 | 2019-12-20 | 浙江新纳材料科技股份有限公司 | Preparation method of hydrophobic white carbon black with controllable particle size and core-shell structure |
| CN110835110A (en) * | 2019-12-12 | 2020-02-25 | 通化双龙硅材料科技有限公司 | Preparation method of precipitated hydrated silicon dioxide |
| CN111634920A (en) * | 2020-06-16 | 2020-09-08 | 福建远翔新材料股份有限公司 | Preparation method of nano silicon dioxide for food anti-caking agent |
| CN112777602A (en) * | 2021-02-25 | 2021-05-11 | 福建正盛无机材料股份有限公司 | Preparation method of precipitated white carbon black for high-performance tire |
| CN114132939A (en) * | 2021-12-27 | 2022-03-04 | 江西省矿产资源保障服务中心 | Method for producing white carbon black by using silicon-implanted silicon ore |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0948611A (en) * | 1995-08-01 | 1997-02-18 | Nippon Silica Ind Co Ltd | Production of fine powder of precipitated silicic acid having abrasiveness |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN101830474A (en) * | 2010-05-17 | 2010-09-15 | 浙江建德建业有机化工有限公司 | Method for preparing white carbon black |
| WO2013092749A1 (en) * | 2011-12-23 | 2013-06-27 | Rhodia Operations | Precipitated-silica production method |
-
2016
- 2016-03-24 CN CN201610170860.9A patent/CN105712361A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0948611A (en) * | 1995-08-01 | 1997-02-18 | Nippon Silica Ind Co Ltd | Production of fine powder of precipitated silicic acid having abrasiveness |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN101830474A (en) * | 2010-05-17 | 2010-09-15 | 浙江建德建业有机化工有限公司 | Method for preparing white carbon black |
| WO2013092749A1 (en) * | 2011-12-23 | 2013-06-27 | Rhodia Operations | Precipitated-silica production method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241816A (en) * | 2016-07-20 | 2016-12-21 | 福建远翔新材料股份有限公司 | A kind of preparation method of silica dioxide delustring agent |
| CN107720762A (en) * | 2017-11-29 | 2018-02-23 | 通化双龙硅材料科技有限公司 | The production method of alkaline white carbon |
| CN110150272A (en) * | 2019-06-05 | 2019-08-23 | 确成硅化学股份有限公司 | A kind of dedicated white carbon black of farm chemical carrier and preparation method thereof |
| CN110589843A (en) * | 2019-10-23 | 2019-12-20 | 浙江新纳材料科技股份有限公司 | Preparation method of hydrophobic white carbon black with controllable particle size and core-shell structure |
| CN110835110A (en) * | 2019-12-12 | 2020-02-25 | 通化双龙硅材料科技有限公司 | Preparation method of precipitated hydrated silicon dioxide |
| CN111634920A (en) * | 2020-06-16 | 2020-09-08 | 福建远翔新材料股份有限公司 | Preparation method of nano silicon dioxide for food anti-caking agent |
| CN111634920B (en) * | 2020-06-16 | 2022-01-18 | 福建远翔新材料股份有限公司 | Preparation method of nano silicon dioxide for food anti-caking agent |
| CN112777602A (en) * | 2021-02-25 | 2021-05-11 | 福建正盛无机材料股份有限公司 | Preparation method of precipitated white carbon black for high-performance tire |
| CN114132939A (en) * | 2021-12-27 | 2022-03-04 | 江西省矿产资源保障服务中心 | Method for producing white carbon black by using silicon-implanted silicon ore |
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Application publication date: 20160629 |