CN103819937A - Aluminum-silicon-coated barium sulfate and preparation method thereof - Google Patents
Aluminum-silicon-coated barium sulfate and preparation method thereof Download PDFInfo
- Publication number
- CN103819937A CN103819937A CN201410105069.0A CN201410105069A CN103819937A CN 103819937 A CN103819937 A CN 103819937A CN 201410105069 A CN201410105069 A CN 201410105069A CN 103819937 A CN103819937 A CN 103819937A
- Authority
- CN
- China
- Prior art keywords
- barium sulfate
- coated
- preparation
- aluminium silicon
- aluminium
- 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.)
- Granted
Links
Images
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of aluminum-silicon-coated barium sulfate. The preparation method is characterized by comprising the following steps: (1) preparation of a coated mixed liquid: mixing sodium silicate liquor and sodium aluminate liquor in a concentration ratio: Al<3+>=0.2mol/L-0.4mol/L, Si<4+>=0.05mol/L-0.15mol/L to obtain the coated mixed liquid; (2) pre-treatment of barium sulfate; and (3) coating a finished product: mixing the barium sulfate emulsion obtained in the step (2) in a proportion of adding 200-500L of the coated mixed liquid obtained in the step (1) into the barium sulfate emulsion per cubic meter, and maintaining the pH value of the liquor in the mixing process over 11; and then, heating, cooling, adjusting the pH to 8.0-8.5, carrying out solid-liquid separation, and washing and drying the solid to obtain an aluminum-silicon-coated barium sulfate product. According to the aluminum-silicon-coated barium sulfate product, the content of barium sulfate is over 95.00%, and the content of aluminum silicate is 1.00-4.00%. D50 is ranged from 0.200 micron to 0.300 micron, the whiteness is over 98.5%, the conductivity is below 70mu s/cm, and the residual value of a 325-mesh sieve is less than 0.05%.
Description
Technical field
The present invention relates to fine inorganic chemical filler preparing technical field, particularly relate to coated barium sulfate of a kind of aluminium silicon and preparation method thereof.
Background technology
In order to improve the dispersiveness of barium sulfate material in organic system, need to be coated processing to barium sulfate surface.Aluminium silicon is coated to be had good heat resistance, is applicable to multiple organic system and obtains widespread use as a kind of inorganic coating material.
General coated operation more easily forms particle agglomeration, needs later stage strengthening to pulverize.The coated process of minimizing is reunited and reduced strengthening crushing process becomes industry research emphasis to the destruction of coating layer.
Therefore, exploitation just has the coated barium sulfate technique of appropriate particle size to become the technical problem of needing solution badly of this area.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of coated barium sulfate product of alkaline system sial hydrolysis growth technique preparation and preparation method thereof that adopts.
The present invention adopts with alkaline system sial hydrolysis growth technique and has prepared coated barium sulfate product, has reduced particle agglomeration, pulverizes without strengthening, has solved the technical problem of coated process due to the particle secondary agglomeration of oxyhydroxide formation.
Specifically, the present invention solves the problems of the technologies described above by following technical solution:
A preparation method for the coated barium sulfate of aluminium silicon, is characterized in that, comprises the steps:
(1) preparation of coated mixed solution: by sodium silicate solution and sodium aluminate solution according to [Al
3+]=0.2mol/L-0.4mol/L, [Si
4+the concentration ratio of]=0.05mol/-0.15mol/L is mixed, and obtains coated mixed solution;
(2) pre-treatment of barium sulfate: the ratio that is 20%-30% according to solid content by barium sulfate is pulled an oar, preferably pulls an oar according to 25% solid content; Adding afterwards alkali to adjust pH value is 10～10.5, carries out afterwards emulsification and obtains barium sulfate emulsion; And
(3) coated finished product: the ratio that the barium sulfate emulsion that step (2) is obtained adds 200-500 to rise the coated mixed solution that step (1) obtains according to every cubic metre of molten emulsion of barium sulfate is mixed, the ratio that preferably adds 300-400 to rise the coated mixed solution that step (1) obtains is mixed, and keeps the pH value of solution in mixing process more than 11; Seal afterwards steam-heated cal(l)andria; Stop heating and carry out coolingly, the pH regulator of cooled mixing solutions, to 8.0-8.5, is carried out to solid-liquid separation afterwards, obtain solid and wash, dry and obtain the coated barium sulfate product of aluminium silicon.
Wherein, described step (1) sodium silicate solution and sodium aluminate solution are according to [Al
3+]=0.3mol/L, [Si
4+the concentration ratio of]=0.1mol/L is mixed.
Wherein, described step (1) sodium aluminate is to prepare by the following method, by metallic aluminium and sodium hydroxide according to Al=0.8mol/L-1.2mol/L, the ratio of NaOH=1.2mol/L～1.5mol/L is reacted, preferable alloy aluminium and sodium hydroxide are according to Al=1.0mol/L, the ratio of NaOH=1.3mol/L is carried out solid-liquid separation after having reacted, and obtains sodium aluminate liquid.
Wherein, described step (1) is prepared temperature of reaction in sodium aluminate process and is controlled at lower than 60 ℃, preferably 50 ℃-60 ℃
Described step (1) is prepared in sodium aluminate process, and metallic aluminium and sodium hydroxide are according to Al=1mol/L, and the concentration of NaOH=1.3mol/L is reacted.
Wherein, described step (2) emulsification is to use emulsification pump to carry out emulsification 1.5-3 hour.
Wherein, the alkali that described step (2) adds is sodium hydroxide.
Wherein, the D50<0.3 micron of barium sulfate in described step (2), whiteness >=98.0%.
Wherein, in described step (3) mixing process by adding sodium hydroxide to keep the pH value of mixing solutions.
Wherein, the pH of the cooled mixing solutions of described step (3) is adjusted to 8.0-8.5 with sulfuric acid.
Wherein, described step (3) heated sealed is that formerly 80 ℃ of heating are warmed up to 105 ℃ of heating gradually; Preferably heat-processed is: 80～85 ℃ × 1h, 90～95 ℃ × 2h, 100～105 ℃ × 1h.
Wherein, described step (3) is cooled to and is less than 90 ℃.
Wherein, before described step (3) solid-liquid separation, stir 0.5-2 hour.
Wherein, described step (3) washing is than being 1:(3-5 according to material quality) add water to carry out heat to wash, preferably to wash temperature be 80～90 ℃ to heat, described oven dry is at 140-160 ℃, to dry 5-7 hour; Preferably at 150 ℃, dry 6 hours.
The present invention also provides a kind of aluminium silicon preparing by above-mentioned preparation method to be coated barium sulfate product, and its barium sulfate content is more than 95.00%, and preferably barium sulfate content is within the scope of 95.00-98.00%; Pure aluminium silicate content is within the scope of 1.00%-4.00%.
Wherein D
50between 0.200 micron-0.300 micron, whiteness is more than 98.5%, and specific conductivity is below 70us/cm, and 325 mesh sieve residual values are less than 0.05%.
Beneficial effect of the present invention is as follows:
(1) the present invention adopts alkaline system sial hydrolysis growth technique to prepare coated barium sulfate product, has reduced particle agglomeration, pulverizes without strengthening, has solved the technical problem of coated process due to the particle secondary agglomeration of oxyhydroxide formation.
(2) barium sulfate product that prepared by the present invention, barium sulfate content is greater than 95.0%, and the content of pure aluminium silicate is between 1%-4%, and whiteness is greater than 98.5%, D
50it is 0.200 micron-0.300 micron.
Accompanying drawing explanation:
Fig. 1: reaction process schema of the present invention;
Fig. 2: the electromicroscopic photograph of sample prepared by the embodiment of the present invention 2;
Embodiment
The method of the preparation of the coated barium sulfate of aluminium silicon of the present invention, realizes by following chemical reaction:
2Al+2NaOH+2H
2O→2NaAlO
2+3H
2↑
BaSO
4+6NaAlO
2+2NaSiO
3+5H
2SO
4
The preparation method who the invention provides the coated barium sulfate of a kind of aluminium silicon, comprises the steps:
(1) preparation of coated mixed solution: by sodium silicate solution and sodium aluminate solution according to aluminium and silicon [Al
3+]=0.2mol/L-0.4mol/L, [Si
4+the ratio of the mol/L of]=(0.05-0.15) is mixed, and obtains coated mixed solution; Preferably, described sodium silicate solution and sodium aluminate solution are according to [Al
3+]=0.3mol/L, [Si
4+the ratio of]=0.1mol/L is mixed; Described sodium aluminate is to prepare by the following method, and by metallic aluminium and sodium hydroxide, according to Al=0.8mol/L-1.2mol/L, the ratio of NaOH=1.3mol/L～1.5mol/L is reacted, and after having reacted, carries out solid-liquid separation, obtains sodium aluminate liquid; Describedly prepare temperature of reaction in sodium aluminate process and be controlled at lower than 60 ℃, preferably 50 ℃-60 ℃; Described preparation in sodium aluminate process, preferable alloy aluminium and sodium hydroxide are according to Al=1mol/L, and the concentration of NaOH=1.3mol/L is reacted.
Above-mentioned sodium silicate solution is prepared in process, has controlled the ratio of aluminium and sodium hydroxide, in the situation that sodium hydroxide is excessive a little, react, the solution obtaining is like this basic solution, is conducive to further reaction.In water glass and sodium aluminate mixing process, control the ratio of silicon and aluminium, particularly control [Al
3+]=0.2mol/L-0.4mol/L, [Si
4+within the scope of]=0.05-0.15mol/L, the particle diameter that is conducive to like this coated prod of controlling last formation meets the requirements.
(2) pre-treatment of barium sulfate: the ratio that is 20%-30% according to solid content by barium sulfate is pulled an oar, preferably carries out slurrying according to 25% solid content; Adding afterwards alkali to adjust pH value is 10～10.5, carries out afterwards emulsification and obtains barium sulfate emulsion; Described emulsification is to use emulsification pump to carry out emulsification 1.5-3 hour; The described alkali adding is sodium hydroxide.
This step is that commercially available barium sulfate is carried out to pretreated process, the D50<0.3 micron of general requirement barium sulfate, whiteness >=98.0%.Barium sulfate is carried out to the strict solid content of controlling in the process of slurrying, be beneficial to further control the content of barium sulfate, control solid content simultaneously and guaranteed the quality of final coated prod in described scope, as whiteness, particle diameter etc.In this step, the pH value of barium sulfate is adjusted to alkalescence, is conducive to carry out the coated of next step simultaneously.
(3) coated finished product: the ratio that the barium sulfate emulsion that step (2) is obtained adds 200-500 to rise the coated mixed solution that step (1) obtains according to every cubic metre of molten emulsion of barium sulfate is mixed, and keeps the pH value of solution in mixing process more than 11; Seal afterwards steam-heated cal(l)andria; Stop carrying out coolingly after heating, the pH regulator of cooled mixing solutions, to 8.0-8.5, is carried out to solid-liquid separation afterwards, obtain solid and wash, dry and obtain the coated barium sulfate product of aluminium silicon; Preferably, in described mixing process by adding sodium hydroxide to keep the pH value of mixing solutions.Preferably, the pH of described cooled mixing solutions is adjusted to 8.0-8.5 with sulfuric acid.Preferably, described heated sealed is that formerly 80 ℃ of heating are warmed up to 105 ℃ of heating gradually; Preferably heat-processed is: 80～85 ℃ × 1h, 90～95 ℃ × 2h, 100～105 ℃ × 1h.Preferably, described in, be cooled to and be less than 90 ℃.Preferably, before described solid-liquid separation, stir 0.5-2 hour, more preferably, described washing is than for 1:(3-5 according to material quality) add water to carry out heat to wash, preferably to wash temperature be 80～90 ℃ to heat, preferably drying is to dry 5-7 hour under 140-160.
The process of above-mentioned coated finished product, the coated mixed solution preparing is pumped in barium sulfate and is coated, particularly control both ratios, the concentration of the solution of preparing based on step (1) and step (2) is controlled mixing process ratio between the two by volume, is beneficial to the coated prod of final fine quality.By sealed reaction, steam heating, also makes the product quality that obtains better.
The present invention also provides a kind of aluminium silicon preparing by aforesaid method to be coated barium sulfate product, its D
50it is 0.200 micron-0.300 micron.Wherein said barium sulfate content 95.0%-98.0%, pure aluminium silicate content is 1.00%-4.00%, water-content is less than 0.10%.The whiteness of the coated barium sulfate product of wherein said aluminium silicon is greater than 98.5%, and specific conductivity is less than 70us/cm.
In the preferred embodiment of one, aluminium silicon of the present invention is coated barium sulfate product preparation method, comprises the steps:
(1) NaAlO
2/ H
2o preparation and mixed solution preparation
Commercially available technical grade aluminium flake is washed down to surface with washing composition, be placed in reaction vessel stirring reaction according to the ratio of Al=1mol/L, NaOH=1.3mol/L, control solution temperature and be less than 60 ℃, reacted rear press filtration and separated, a small amount of residue is abandoned, and clear liquor enters batching operation.
By the sodium aluminate solution of commercially available sodium silicate solution and preparation according to [Al
3+]=0.30mol/L, [Si
4+the ratio of]=0.10mol/L mixes stand-by.
(2) coated processing and moulding
By the BaSO after synthesis of detergent
4(D50<0.3 micron, whiteness>=98.0%), according to the ratio making beating of solid content 25%, adds NaOH to adjust pH10～10.5, uses emulsification pump dispersion and emulsion 2 hours, stops emulsification, maintains stirring.
Require the ratio that adds 200-500 to rise the coated mixed solution that step (1) obtains according to every cubic metre of molten emulsion of barium sulfate to pump into the mixing solutions preparing according to different covering amounts, detect pH value of solution and be greater than 11, if desired supplementary NaOH.
Confined reaction pot afterwards, opens steam heating, controls temperature 80～85 ℃ × 1h, 90～95 ℃ × 2h, 100～105 ℃ × 1h, stops heating, and chuck is cooled to and is less than 90 ℃.
Under stirring, (add volume 98% sulfuric acid to prepare with trisome ponding with 1+3 sulfuric acid, concentration is about about 4.5mol/L) be neutralized to pH8.0～8.5, maintain and stir press filtration separation after 1 hour, 80～90 ℃ of heat of 1:4 material-water ratio are washed three times, wash in mother liquor and discharge, 150 ℃ × 6h of filter cake is dried, and obtains the coated barium sulfate product of aluminium silicon after crushing packing.
Embodiment
First when, barium sulfate preparation process in embodiment below and product analyses, determinator and measuring method used is described as follows:
Industry aluminium flake: aluminium content is >=90%.
Aluminum cleaning agent: Nantong Rui Ao Chemical Co., Ltd.
Technical grade hydrated barta: Ba (OH)
2content>=98%.
Barium sulfate: D50<0.3 micron, whiteness >=98.0%.
1+3 sulfuric acid: add 98% sulfuric acid of a volume to prepare with trisome ponding, concentration is about 4.5mol/L left and right
What use about part measuring method in barium sulfate product analysis is standard SN/T0480-1995(outlet barite analytical procedure) in measuring method; Specifically, barium sulfate content is measured the method adopting in SN/T0480.5-1995.
The measuring brightness instrument (adopt 200 mesh sieves, measure after 105 ℃ of oven dry) that the model that measuring brightness adopts Jinan MICHAEL DRAKE Instrument Ltd. to produce is DRK103A is measured according to disclosed method in SN/T0480.12-1995.
The mensuration of product pattern: JSM-6490LV type scanning electronic microscope, NEC company system.
Particle size determination: JSM-6490LV type scanning electronic microscope, NEC company system.
PH pH-value determination pH adopts PHS-3C type precision acidity meter, and by Shanghai, precision instrumentation company manufactures.
The mensuration of 325 mesh sieve residual values: adopt the method for SN/T0480.2-1995 to measure;
The mensuration of specific conductivity: conductivity measuring instrument, Guangzhou De Manyi Instrument Ltd., DDS-11A.
Embodiment 1
Shown in the process flow sheet of lower combination Fig. 1, illustrate that the present invention prepares the coated barium sulfate preparation method of aluminium silicon.Described preparation method comprises the steps:
(1) preparation of coated mixed solution
By commercially available technical grade aluminium flake aluminum cleaning agent clean surface, according to the ratio of Al=0.8mol/L, NaOH=1.5mol/L, aluminium flake and sodium hydroxide are placed in to 5m
3reactor in, stirring reaction, controlling solution temperature is 55 ℃ following (being less than 60 ℃), react rear press filtration separation, and a small amount of residue obtaining is abandoned, the clear liquor obtaining is sodium aluminate solution, stand-by.
By the sodium aluminate solution of commercially available sodium silicate solution and above-mentioned preparation according to [Al
3+]=0.30mol/L, [Si
4+the ratio of]=0.10mol/L mixes, and obtains coated mixed solution, stand-by.
(2) pre-treatment of barium sulfate
By BaSO
4(D50=0.2 micron, whiteness>=98.0%), according to the ratio making beating of solid content 20%, adds NaOH to adjust pH10.3, uses emulsification pump dispersion and emulsion 1.5 hours, stops emulsification, maintains stirring.
(3) coated processing and moulding
Require to add the ratio of the coated mixed solution that 235 liters of steps (1) obtain to pump into the mixing solutions preparing according to every cubic metre of molten emulsion of barium sulfate according to different covering amounts, detecting pH value of solution is that 11.2(is greater than 11), supplement if desired NaOH.
Confined reaction pot afterwards, opens steam heating, controls temperature 80 ℃ × 1h, 90 ℃ × 2h, 100 ℃ × 1h, stops heating, and chuck is cooled to 85 ℃ (being less than 90 ℃).
Under stirring, be neutralized to pH8.2 with 1+3 sulfuric acid, maintain and stir press filtration separation after 1 hour, 85 ℃ of heat of 1:4 material-water ratio are washed three times, wash in mother liquor and discharge, 150 ℃ × 6h of filter cake is dried, and obtains the coated barium sulfate product 1# of aluminium silicon after crushing packing, it is carried out to barium sulfate content, pure aluminium silicate content, whiteness, whiteness, particle diameter, specific conductivity, the mensuration of water-content and 325 mesh sieve residual values, measurement result is in table 1, and electromicroscopic photograph is shown in Fig. 2.
Embodiment 2
Described aluminium silicon is coated barium sulfate preparation method, comprises the steps:
(1) preparation of coated mixed solution
By commercially available technical grade aluminium flake aluminum cleaning agent clean surface, according to the ratio of Al=1.0mol/L, NaOH=1.3mol/L, aluminium flake and sodium hydroxide are placed in to 5m
3reactor in, stirring reaction, controlling solution temperature is 58 ℃ following (being less than 60 ℃), react rear press filtration separation, and a small amount of residue obtaining is abandoned, the clear liquor obtaining is sodium aluminate solution, stand-by.
By the sodium aluminate solution of commercially available sodium silicate solution and above-mentioned preparation according to [Al
3+]=0.30mol/L, [Si
4+the ratio of]=0.10mol/L mixes, and obtains coated mixed solution, stand-by.
(2) pre-treatment of barium sulfate
By BaSO
4(D50=0.25 micron, whiteness>=98.0%), according to the ratio making beating of solid content 25%, adds NaOH to adjust pH10.3, uses emulsification pump dispersion and emulsion 2 hours, stops emulsification, maintains stirring.
(3) coated processing and moulding
Require to add the ratio of the coated mixed solution that 355 liters of steps (1) obtain to pump into the mixing solutions preparing according to every cubic metre of molten emulsion of barium sulfate according to different covering amounts, detecting pH value of solution is that 11.2(is greater than 11), supplement if desired NaOH.
Confined reaction pot afterwards, opens steam heating, controls temperature 83 ℃ × 1h, 93 ℃ × 2h, 103 ℃ × 1h, stops heating, and chuck is cooled to 88 ℃ of (being less than 90 ℃) (being less than 90 ℃).
Under stirring, be neutralized to pH8.2 with 1+3 sulfuric acid, maintain and stir press filtration separation after 1 hour, 85 ℃ of heat of 1:4 material-water ratio are washed three times, wash in mother liquor and discharge, 150 ℃ × 6h of filter cake is dried, and obtains the coated barium sulfate product 2# of aluminium silicon after crushing packing, it is carried out to barium sulfate content, pure aluminium silicate content, whiteness, whiteness, particle diameter, specific conductivity, the mensuration of water-content and 325 mesh sieve residual values, measurement result is in table 1, and electromicroscopic photograph is shown in Fig. 2.
Embodiment 3
(1) preparation of coated mixed solution
By commercially available technical grade aluminium flake aluminum cleaning agent clean surface, according to the ratio of Al=1.2mol/L, NaOH=1.2mol/L, aluminium flake and sodium hydroxide are placed in to 5m
3reactor in, stirring reaction, controlling solution temperature is below 60 ℃, react rear press filtration separation, and a small amount of residue obtaining is abandoned, the clear liquor obtaining is sodium aluminate solution, stand-by.
By the sodium aluminate solution of commercially available sodium silicate solution and above-mentioned preparation according to [Al
3+]=0.40mol/L, [Si
4+the ratio of]=0.05mol/L mixes, and obtains coated mixed solution, stand-by.
(2) pre-treatment of barium sulfate
By BaSO
4(D50=0.2 micron, whiteness>=98.0%), according to the ratio making beating of solid content 30%, adds NaOH to adjust pH10.5, uses emulsification pump dispersion and emulsion 3 hours, stops emulsification, maintains stirring.
(3) coated processing and moulding
Require to add the ratio of the coated mixed solution that 470 liters of steps (1) obtain to pump into the mixing solutions preparing according to every cubic metre of molten emulsion of barium sulfate according to different covering amounts, detecting pH value of solution is that 11.3(is greater than 11), when pH supplements NaOH lower than 11.0 time to maintain pH more than 11.
Confined reaction pot afterwards, opens steam heating, controls temperature 85 ℃ × 1h, 95 ℃ × 2h, 105 ℃ × 1h, stops heating, and chuck is cooled to 90 ℃.
Under stirring, be neutralized to pH8.2 with 1+3 sulfuric acid, maintain and stir press filtration separation after 1 hour, 85 ℃ of heat of 1:4 material-water ratio are washed three times, wash in mother liquor and discharge, 150 ℃ × 6h of filter cake is dried, and obtains the coated barium sulfate product 3# of aluminium silicon after crushing packing, and it is carried out to barium sulfate content, pure aluminium silicate content, whiteness, whiteness, particle diameter, specific conductivity, the mensuration of water-content and 325 mesh sieve residual values, measurement result is in table 1.
The barium sulfate product property testing result that table 1 embodiment 1-3 prepares
| Project | 1# | 2# | 3# |
| BaSO 4Content (%) | 97.61 | 96.81 | 95.74 |
| Pure aluminium silicate (%) | 1.94 | 2.87 | 3.90 |
| Whiteness (%) | >98.5 | >98.5 | >98.5 |
| D 50（μm） | 0.243 | 0.259 | 0.280 |
| Specific conductivity (us/cm) | <70 | <70 | <70 |
| H 2O（%） | <0.10 | <0.10 | <0.10 |
| 325 mesh sieve residual values (%) | <0.05 | <0.05 | <0.05 |
Show by the result in upper table, in the coated barium sulfate product of aluminium silicon that embodiment of the present invention 1-3 prepares, barium sulfate content is more than 95.00%, and barium sulfate content is all within the scope of 95.00-98.00%; Pure aluminium silicate content is within the scope of 1.00%-4.00%, and water-content is all lower than 0.10%; D
50between 0.200 micron-0.300 micron, whiteness is more than 98.5%, and specific conductivity is below 70us/cm.The coated barium sulfate of aluminium silicon prepared by above-mentioned digital proof the present invention has high whiteness, the feature that particle diameter is little.
The present invention has carried out above-mentioned description to some preferred implementation and embodiment, to help the public to use suitable experimental technique in enforcement process of the present invention, obtain good experiment effect, this does not get rid of the experimental technique being equal to of not enumerating in the present invention also can implement the present invention.It will be appreciated by those skilled in the art that the present invention is except specifically described mode, can also be applicable to distortion and revise.Should be understood that, the present invention includes all these distortion and modification.Further, denomination of invention, title or similar part are in order to strengthen the public to understanding herein, should not to be regarded as limiting the scope of the present invention.
Make a general survey of whole specification sheets and claims, unless context needs, otherwise word " comprises ", " comprising " and similar word, and the implication that is interpreted as comprising but not the implication got rid of that is to say, look like for " including, but are not limited to ".
Claims (15)
1. a preparation method for the coated barium sulfate of aluminium silicon, is characterized in that, comprises the steps:
(1) preparation of coated mixed solution: by sodium silicate solution and sodium aluminate solution according to [Al
3+]=0.2mol/L-0.4mol/L, [Si
4+the concentration ratio of]=0.05mol/-0.15mol/L is mixed, and obtains coated mixed solution;
(2) pre-treatment of barium sulfate: the ratio that is 20%-30% according to solid content by barium sulfate is pulled an oar, preferably pulls an oar according to 25% solid content; Adding afterwards alkali to adjust pH value is 10～10.5, carries out afterwards emulsification and obtains barium sulfate emulsion; And
(3) coated finished product: the ratio that the barium sulfate emulsion that step (2) is obtained adds 200-500 to rise the coated mixed solution that step (1) obtains according to every cubic metre of molten emulsion of barium sulfate is mixed, the ratio that preferably adds 300-400 to rise the coated mixed solution that step (1) obtains is mixed, and keeps the pH value of solution in mixing process more than 11; Seal afterwards steam-heated cal(l)andria; Stop heating and carry out coolingly, the pH regulator of cooled mixing solutions, to 8.0-8.5, is carried out to solid-liquid separation afterwards, obtain solid and wash, dry and obtain the coated barium sulfate product of aluminium silicon.
2. the preparation method of the coated barium sulfate of aluminium silicon according to claim 1, wherein said step (1) sodium silicate solution and sodium aluminate solution are according to [Al
3+]=0.3mol/L, [Si
4+the concentration ratio of]=0.1mol/L is mixed.
3. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1 or 2, described step (1) sodium aluminate is to prepare by the following method, by metallic aluminium and sodium hydroxide according to Al=0.8mol/L-1.2mol/L, the ratio of NaOH=1.2mol/L～1.5mol/L is reacted, preferable alloy aluminium and sodium hydroxide are according to Al=1.0mol/L, the ratio of NaOH=1.3mol/L is carried out solid-liquid separation after having reacted, and obtains sodium aluminate liquid.
4. the preparation method of the coated barium sulfate of aluminium silicon according to claim 3, described step (1) is prepared temperature of reaction in sodium aluminate process and is controlled at lower than 60 ℃, preferably 50 ℃-60 ℃.
5. the preparation method of the coated barium sulfate of aluminium silicon according to claim 4, described step (1) is prepared in sodium aluminate process, and metallic aluminium and sodium hydroxide are according to Al=1mol/L, and the concentration of NaOH=1.3mol/L is reacted.
6. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-5 any one, described step (2) emulsification is to use emulsification pump to carry out emulsification 1.5-3 hour.
7. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-6 any one, the alkali that described step (2) adds is sodium hydroxide.
8. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-7 any one, in described step (3) mixing process by adding sodium hydroxide to keep the pH value of mixing solutions.
9. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-8 any one, the pH of the cooled mixing solutions of described step (3) is adjusted to 8.0-8.5 with sulfuric acid.
10. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-9 any one, described step (3) heated sealed is that formerly 80 ℃ of heating are warmed up to 105 ℃ of heating gradually; Preferably heat-processed is: 80～85 ℃ × 1h, 90～95 ℃ × 2h, 100～105 ℃ × 1h.
11. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-10 any one, and described step (3) is cooled to and is less than 90 ℃.
12. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-11 any one, before described step (3) solid-liquid separation, stirs 0.5-2 hour.
13. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 1-12 any one, described step (3) washing is than being 1:(3-5 according to material quality) add water to carry out heat to wash, it is 80～90 ℃ that preferred heat is washed temperature, and described oven dry is to dry 5-7 hour at 140-160 ℃; Preferably at 150 ℃, dry 6 hours.
14. 1 kinds of coated barium sulfate products of the aluminium silicon preparing by preparation method described in claim 1-13 any one, its barium sulfate content is more than 95.00%, and preferably barium sulfate content is within the scope of 95.00-98.00%; Pure aluminium silicate content is within the scope of 1.00%-4.00%.
15. aluminium silicon as claimed in claim 14 are coated barium sulfate product, its D
50between 0.200 micron-0.300 micron, whiteness is more than 98.5%, and specific conductivity is below 70us/cm, and 325 mesh sieve residual values are less than 0.05%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105069.0A CN103819937B (en) | 2014-03-20 | 2014-03-20 | Coated barium sulfate of a kind of aluminium silicon and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105069.0A CN103819937B (en) | 2014-03-20 | 2014-03-20 | Coated barium sulfate of a kind of aluminium silicon and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103819937A true CN103819937A (en) | 2014-05-28 |
| CN103819937B CN103819937B (en) | 2016-03-16 |
Family
ID=50755243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410105069.0A Active CN103819937B (en) | 2014-03-20 | 2014-03-20 | Coated barium sulfate of a kind of aluminium silicon and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103819937B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101534A (en) * | 1986-08-07 | 1988-02-17 | 上海京华化工厂 | The preparation method of water dispersing lide powder pigment |
| US20030124048A1 (en) * | 2000-05-31 | 2003-07-03 | Solvay Barium Strontium Gmbh | Micronized barium sulfate |
| CN101250336A (en) * | 2008-04-10 | 2008-08-27 | 上海安亿纳米材料有限公司 | Barium sulfate based polybasic composite white pigments and method for preparing same |
| CN102051073A (en) * | 2010-12-20 | 2011-05-11 | 昆明理工大学 | Surface-modified titanium white powder and preparation method thereof |
| WO2013003137A1 (en) * | 2011-06-28 | 2013-01-03 | E.I. Du Pont De Nemours And Company | Treated inorganic particle |
| CN103130260A (en) * | 2013-03-19 | 2013-06-05 | 冉金友 | Production method of barium sulfate |
-
2014
- 2014-03-20 CN CN201410105069.0A patent/CN103819937B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101534A (en) * | 1986-08-07 | 1988-02-17 | 上海京华化工厂 | The preparation method of water dispersing lide powder pigment |
| US20030124048A1 (en) * | 2000-05-31 | 2003-07-03 | Solvay Barium Strontium Gmbh | Micronized barium sulfate |
| CN101250336A (en) * | 2008-04-10 | 2008-08-27 | 上海安亿纳米材料有限公司 | Barium sulfate based polybasic composite white pigments and method for preparing same |
| CN102051073A (en) * | 2010-12-20 | 2011-05-11 | 昆明理工大学 | Surface-modified titanium white powder and preparation method thereof |
| WO2013003137A1 (en) * | 2011-06-28 | 2013-01-03 | E.I. Du Pont De Nemours And Company | Treated inorganic particle |
| CN103130260A (en) * | 2013-03-19 | 2013-06-05 | 冉金友 | Production method of barium sulfate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103819937B (en) | 2016-03-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100460328C (en) | Technical process for producing chloride aluminum | |
| CN100411991C (en) | Preparation method of aluminium hydroxide micro powder | |
| CN104556177B (en) | Flake nano γ-Al2O3 and preparation method thereof | |
| WO2010078821A1 (en) | Method for preparing subsphaeroidal barium sulfate by sulfuric acid process and its use in copper foil substrate | |
| CN106379924A (en) | Nano magnesium-aluminum hydrotalcite and preparation method thereof | |
| CN108997788A (en) | The preparation method of high covering power titanium dioxide | |
| CN107745133A (en) | A kind of inexpensive environment-friendly preparation method thereof of Nanometer Copper | |
| CN104326480A (en) | Method for preparing micro-hole calcium silicate by adopting water glass and lime emulsion | |
| CN103693671B (en) | A kind of submicron platy barium sulfate and preparation method thereof | |
| CN114921851A (en) | Calcium carbonate whisker prepared by carbide slag carbonization and preparation method thereof | |
| CN112960685A (en) | Preparation method of nano calcium carbonate for filling hard PVC (polyvinyl chloride) | |
| CN103936013B (en) | A kind of method preparing white carbon black slurries | |
| CN102441675A (en) | Preparation method for high-crystallinity silver powder | |
| CN105016343B (en) | A kind of method that utilization aluminous fly-ash prepares hydrophabic silica | |
| CN103466640B (en) | A kind of method reducing the standby white carbon black specific surface area BET of sulfuric acid precipitation legal system | |
| CN107573542B (en) | High-jet-flow hydrophobic starch and preparation method thereof | |
| CN104556160B (en) | A kind of γ-Al2o3nanocrystal and preparation method thereof | |
| CN104988576B (en) | The preparation method of alkali magnesium sulfate crystal whisker | |
| CN112661164A (en) | Method for preparing calcium silicate hydrate by using waste liquid as raw material | |
| CN103819937B (en) | Coated barium sulfate of a kind of aluminium silicon and preparation method thereof | |
| CN110255619B (en) | Method for preparing molybdenum sulfide with three-dimensional hollow structure based on up-conversion nanoparticles | |
| CN112456525A (en) | Preparation method of boehmite with low water absorption | |
| CN103864129A (en) | High-dispersion barium sulfate and preparation method thereof | |
| CN103641145A (en) | High-whiteness barium sulfate and preparation method thereof | |
| CN114249343B (en) | Production method of calcium hydroxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Free format text: FORMER OWNER: SHENZHEN HAOYITONG INVESTMENT + DEVELOPMENT CO., LTD. Effective date: 20141215 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20141215 Address after: 561206 Guizhou city of Anshun province Zhenning County small town Applicant after: Beijing Wankun Jiahong Science and Technology Development Co., Ltd. Address before: 561206 Guizhou city of Anshun province Zhenning County small town Applicant before: Beijing Wankun Jiahong Science and Technology Development Co., Ltd. Applicant before: Shenzhen Haoyitong Investment & Development Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |