CN103819937B - Coated barium sulfate of a kind of aluminium silicon and preparation method thereof - Google Patents
Coated barium sulfate of a kind of aluminium silicon and preparation method thereof Download PDFInfo
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- CN103819937B CN103819937B CN201410105069.0A CN201410105069A CN103819937B CN 103819937 B CN103819937 B CN 103819937B CN 201410105069 A CN201410105069 A CN 201410105069A CN 103819937 B CN103819937 B CN 103819937B
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Abstract
The invention discloses the preparation method of the coated barium sulfate of a kind of aluminium silicon, it is characterized in that, comprise the steps: the preparation of (1) 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 mixes, and obtains coated mixed solution; (2) pre-treatment of barium sulfate; And (3) coated finished product: barium sulfate emulsion step (2) obtained adds according to every cubic metre of molten emulsion of barium sulfate the ratio that 200-500 rises the coated mixed solution that step (1) obtains and mixes, and keeps the pH value of solution in mixing process more than 11; Carry out afterwards heating, cooling, pH regulator is to 8.0-8.5, and solid-liquid separation, washs obtaining solid, dry and obtain the coated barium sulfate product of aluminium silicon.The coated barium sulfate product of described aluminium silicon, its barium sulfate content is more than 95.00%; Alumina silicate content is within the scope of 1.00%-4.00%.D
50between 0.200 micron-0.300 micron, whiteness is more than 98.5%, and specific conductivity is at below 70us/cm, and 325 mesh sieve residual values are 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 carry out coated process to barium sulfate surface.Aluminium silicon is coated has good heat resistance as a kind of inorganic coating material, be applicable to multiple organic system and obtain widespread use.
General coated operation more easily forms particle agglomeration, needs the later stage to strengthen and pulverizes.Reduce coated process to reunite and reduce the strengthening destruction of crushing process to coating layer and become industry research emphasis.
Therefore, exploitation just has the coated barium sulfate technique of appropriate particle size to become the technical problem needing solution badly of this area.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of alkaline system sial hydrolysis growth technique that adopts and prepares coated barium sulfate product and preparation method thereof.
Employing alkaline system sial hydrolysis growth technique of the present invention has prepared coated barium sulfate product, decreases particle agglomeration, pulverizes, solve the technical problem of the particle secondary agglomeration that coated process is formed due to oxyhydroxide without the need to strengthening.
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, comprise 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 mixes, and obtains coated mixed solution;
(2) pre-treatment of barium sulfate: barium sulfate is pulled an oar according to the ratio that solid content is 20%-30%, preferably pulls an oar according to the solid content of 25%; Adding alkali adjusted to ph is afterwards 10 ~ 10.5, carries out emulsification afterwards and obtains barium sulfate emulsion; And
(3) coated finished product: barium sulfate emulsion step (2) obtained adds according to every cubic metre of molten emulsion of barium sulfate the ratio that 200-500 rises the coated mixed solution that step (1) obtains and mixes, preferably add the ratio that 300-400 rises the coated mixed solution that step (1) obtains to mix, in mixing process, keep the pH value of solution more than 11; Carry out sealing steam-heated cal(l)andria afterwards; Stop heating cooling, by the pH regulator of cooled mixing solutions to 8.0-8.5, carry out solid-liquid separation afterwards, obtain solid and carry out washing, 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 mixes.
Wherein, described step (1) sodium aluminate prepares 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 carries 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 lower than 60 DEG C, preferably 50 DEG C-60 DEG C
Described step (1) is prepared in sodium aluminate process, and metallic aluminium and sodium hydroxide react according to the concentration of Al=1mol/L, NaOH=1.3mol/L.
Wherein, described step (2) emulsification uses 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, the pH value of mixing solutions is kept in described step (3) mixing process by adding sodium hydroxide.
Wherein, the pH sulfuric acid of described step (3) cooled mixing solutions carries out being adjusted to 8.0-8.5.
Wherein, described step (3) heated sealed is warmed up to 105 DEG C of heating gradually in first 80 DEG C of heating; Preferred heat-processed is: 80 ~ 85 DEG C × 1h, 90 ~ 95 DEG C × 2h, 100 ~ 105 DEG C × 1h.
Wherein, described step (3) is cooled to and is less than 90 DEG C.
Wherein, stirring 0.5-2 hour is carried out before described step (3) solid-liquid separation.
Wherein, described step (3) washing is than for 1:(3-5 according to material quality) add water and carry out heat and wash, it is 80 ~ 90 DEG C that preferred heat washes temperature, and described oven dry is at 140-160 DEG C, dry 5-7 hour; Preferably dry 6 hours at 150 DEG C.
The present invention also provides a kind of coated barium sulfate product of aluminium silicon prepared by above-mentioned preparation method, and its barium sulfate content is more than 95.00%, and preferably barium sulfate content is within the scope of 95.00-98.00%; Alumina 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 at 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, decreases particle agglomeration, pulverizes, solve the technical problem of the particle secondary agglomeration that coated process is formed due to oxyhydroxide without the need to strengthening.
(2) barium sulfate product prepared of 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 illustrates:
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, is realized by following chemical reaction:
2Al+2NaOH+2H
2O→2NaAlO
2+3H
2↑
BaSO
4+6NaAlO
2+2NaSiO
3+5H
2SO
4
The invention provides the preparation method of the coated barium sulfate of a kind of aluminium silicon, comprise 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+]=(0.05-0.15) ratio of mol/L mixes, 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 mixing of]=0.1mol/L; Described sodium aluminate prepares by the following method, metallic aluminium and sodium hydroxide reacted according to the ratio of Al=0.8mol/L-1.2mol/L, NaOH=1.3mol/L ~ 1.5mol/L, carry out solid-liquid separation after having reacted, obtain sodium aluminate liquid; Describedly prepare temperature of reaction in sodium aluminate process and control lower than 60 DEG C, preferably 50 DEG C-60 DEG C; Describedly prepare in sodium aluminate process, preferable alloy aluminium and sodium hydroxide react according to the concentration of Al=1mol/L, NaOH=1.3mol/L.
Above-mentionedly be prepared in process to sodium silicate solution, control the ratio of aluminium and sodium hydroxide, react when sodium hydroxide is excessive a little, the solution obtained like this is basic solution, is conducive to further reaction.To in water glass and sodium aluminate mixing process, control the ratio of Silicified breccias, particularly control [Al
3+]=0.2mol/L-0.4mol/L, [Si
4+within the scope of]=0.05-0.15mol/L, the particle diameter being conducive to controlling the last coated prod formed like this meets the requirements.
(2) pre-treatment of barium sulfate: pulled an oar according to the ratio that solid content is 20%-30% by barium sulfate, preferably carries out slurrying according to the solid content of 25%; Adding alkali adjusted to ph is afterwards 10 ~ 10.5, carries out emulsification afterwards and obtains barium sulfate emulsion; Described emulsification uses emulsification pump to carry out emulsification 1.5-3 hour; The described alkali added is sodium hydroxide.
This step carries out pretreated process to commercially available barium sulfate, the D50<0.3 micron of general requirement barium sulfate, whiteness >=98.0%.Carry out barium sulfate strictly controlling solid content in the process of slurrying, be beneficial to the content controlling barium sulfate further, control the quality that solid content ensure that final coated prod in described scope, as whiteness, particle diameter etc. simultaneously.In this step the pH value of barium sulfate is adjusted to alkalescence simultaneously, is conducive to carrying out the coated of next step.
(3) coated finished product: barium sulfate emulsion step (2) obtained adds according to every cubic metre of molten emulsion of barium sulfate the ratio that 200-500 rises the coated mixed solution that step (1) obtains and mixes, and keeps the pH value of solution in mixing process more than 11; Carry out sealing steam-heated cal(l)andria afterwards; Cool after stopping heating, by the pH regulator of cooled mixing solutions to 8.0-8.5, carry out solid-liquid separation afterwards, obtain solid and carry out washing, dry and obtain the coated barium sulfate product of aluminium silicon; Preferably, the pH value of mixing solutions is kept in described mixing process by adding sodium hydroxide.Preferably, the pH sulfuric acid of described cooled mixing solutions carries out being adjusted to 8.0-8.5.Preferably, described heated sealed is warmed up to 105 DEG C of heating gradually in first 80 DEG C of heating; Preferred heat-processed is: 80 ~ 85 DEG C × 1h, 90 ~ 95 DEG C × 2h, 100 ~ 105 DEG C × 1h.Preferably, be cooled to described in and be less than 90 DEG C.Preferably, carry out stirring 0.5-2 hour before described solid-liquid separation, more preferably, described washing is than for 1:(3-5 according to material quality) add water and carry out heat and wash, it is 80 ~ 90 DEG C that preferred heat washes temperature, and preferably drying is dry 5-7 hour under 140-160.
The process of above-mentioned coated finished product, the coated mixed solution prepared is pumped into carry out in barium sulfate coated, ratio both particularly controlling, the concentration of the solution prepared 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.
Present invention also offers a kind of coated barium sulfate product of aluminium silicon prepared by aforesaid method, its D
50it is 0.200 micron-0.300 micron.Wherein said barium sulfate content 95.0%-98.0%, alumina silicate content is 1.00%-4.00%, and 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, the coated barium sulfate product preparation method of aluminium silicon of the present invention, comprises the steps:
(1) NaAlO
2/ H
2o preparation and Compound mixed solution
Commercially available technical grade aluminium flake washing composition is washed down surface, is placed in reaction vessel according to the ratio of Al=1mol/L, NaOH=1.3mol/L, stirring reaction, control solution temperature and be less than 60 DEG C, reacted rear press filtration to be separated, a small amount of residue is abandoned, and clear liquor enters dispensing 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 process and shaping
By the BaSO after synthesis of detergent
4(D50<0.3 micron, whiteness>=98.0%) pulls an oar according to the ratio of solid content 25%, adds NaOH and adjusts pH10 ~ 10.5, with emulsification pump dispersion and emulsion 2 hours, stops emulsification, maintains and stir.
Require that adding according to every cubic metre of molten emulsion of barium sulfate the ratio that 200-500 rises the coated mixed solution that step (1) obtains pumps into the mixing solutions prepared, and detects pH value of solution and is greater than 11, if desired supplementary NaOH according to different covering amount.
Confined reaction pot afterwards, opens steam heating, control temperature 80 ~ 85 DEG C × 1h, 90 ~ 95 DEG C × 2h, 100 ~ 105 DEG C × 1h, and stop heating, chuck is cooled to and is less than 90 DEG C.
(add volume 98% sulfuric acid with three volumes water to prepare with 1+3 sulfuric acid under stirring, concentration is about about 4.5mol/L) be neutralized to pH8.0 ~ 8.5, maintain stirring press filtration separation after 1 hour, 1:4 material-water ratio 80 ~ 90 DEG C of heat wash three times, wash in mother liquor and discharge, filter cake 150 DEG C × 6h is dried, and obtains the coated barium sulfate product of aluminium silicon after crushing packing.
Embodiment
First, when analyzing barium sulfate preparation process in embodiment below and product, determinator used and measuring method are 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: 98% sulfuric acid adding a volume with three volumes water prepares, and concentration is about about 4.5mol/L
Use standard SN/T0480-1995(to export barite analytical procedure about the part measuring method in barium sulfate product analysis) in measuring method; Specifically, barium sulfate content measures the method adopted in SN/T0480.5-1995.
The model that measuring brightness adopts Jinan MICHAEL DRAKE Instrument Ltd. to produce is that the measuring brightness instrument (adopt 200 mesh sieves, dry rear mensuration for 105 DEG C) of DRK103A measures according to method disclosed in SN/T0480.12-1995.
The mensuration of product pattern: JSM-6490LV type scanning electronic microscope, NEC Inc..
Particle size determination: JSM-6490LV type scanning electronic microscope, NEC Inc..
PH value measures and adopts PHS-3C type precision acidity meter, is manufactured by Shanghai precision instrumentation company.
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
Illustrate shown in the process flow sheet of lower composition graphs 1 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 5m
3reactor in, stirring reaction, control solution temperature be less than 55 DEG C (being less than 60 DEG C), reacted rear press filtration separation, abandoned by a small amount of residue obtained, the clear liquor obtained 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%) pulls an oar according to the ratio of solid content 20%, adds NaOH and adjusts pH10.3, with emulsification pump dispersion and emulsion 1.5 hours, stops emulsification, maintains and stir.
(3) coated process and shaping
Require that the ratio adding the coated mixed solution that 235 liters of steps (1) obtain according to every cubic metre of molten emulsion of barium sulfate pumps into the mixing solutions prepared according to different covering amount, detecting pH value of solution is that 11.2(is greater than 11), supplement NaOH if desired.
Confined reaction pot afterwards, opens steam heating, control temperature 80 DEG C × 1h, 90 DEG C × 2h, 100 DEG C × 1h, and stop heating, chuck is cooled to 85 DEG C (being less than 90 DEG C).
PH8.2 is neutralized to 1+3 sulfuric acid under stirring, maintain stirring press filtration separation after 1 hour, 1:4 material-water ratio 85 DEG C of heat wash three times, wash in mother liquor and discharge, filter cake 150 DEG C × 6h is dried, and obtains the coated barium sulfate product 1# of aluminium silicon after crushing packing, barium sulfate content, alumina silicate content, whiteness, whiteness, particle diameter, specific conductivity are carried out to it, 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
The coated barium sulfate preparation method of described aluminium silicon, 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 5m
3reactor in, stirring reaction, control solution temperature be less than 58 DEG C (being less than 60 DEG C), reacted rear press filtration separation, abandoned by a small amount of residue obtained, the clear liquor obtained 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%) pulls an oar according to the ratio of solid content 25%, adds NaOH and adjusts pH10.3, with emulsification pump dispersion and emulsion 2 hours, stops emulsification, maintains and stir.
(3) coated process and shaping
Require that the ratio adding the coated mixed solution that 355 liters of steps (1) obtain according to every cubic metre of molten emulsion of barium sulfate pumps into the mixing solutions prepared according to different covering amount, detecting pH value of solution is that 11.2(is greater than 11), supplement NaOH if desired.
Confined reaction pot afterwards, opens steam heating, control temperature 83 DEG C × 1h, 93 DEG C × 2h, 103 DEG C × 1h, and stop heating, chuck is cooled to 88 DEG C of (being less than 90 DEG C) (being less than 90 DEG C).
PH8.2 is neutralized to 1+3 sulfuric acid under stirring, maintain stirring press filtration separation after 1 hour, 1:4 material-water ratio 85 DEG C of heat wash three times, wash in mother liquor and discharge, filter cake 150 DEG C × 6h is dried, and obtains the coated barium sulfate product 2# of aluminium silicon after crushing packing, barium sulfate content, alumina silicate content, whiteness, whiteness, particle diameter, specific conductivity are carried out to it, 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 5m
3reactor in, stirring reaction, control solution temperature be less than 60 DEG C, react rear press filtration separation, abandoned by a small amount of residue obtained, the clear liquor obtained 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%) pulls an oar according to the ratio of solid content 30%, adds NaOH and adjusts pH10.5, with emulsification pump dispersion and emulsion 3 hours, stops emulsification, maintains and stir.
(3) coated process and shaping
Require that the ratio adding the coated mixed solution that 470 liters of steps (1) obtain according to every cubic metre of molten emulsion of barium sulfate pumps into the mixing solutions prepared according to different covering amount, detect pH value of solution be that 11.3(is greater than 11), when pH lower than 11.0 time supplement NaOH to maintain pH more than 11.
Confined reaction pot afterwards, opens steam heating, control temperature 85 DEG C × 1h, 95 DEG C × 2h, 105 DEG C × 1h, and stop heating, chuck is cooled to 90 DEG C.
PH8.2 is neutralized to 1+3 sulfuric acid under stirring, maintain stirring press filtration separation after 1 hour, 1:4 material-water ratio 85 DEG C of heat wash three times, wash in mother liquor and discharge, filter cake 150 DEG C × 6h is dried, and obtains the coated barium sulfate product 3# of aluminium silicon, carry out barium sulfate content, alumina silicate content, whiteness, whiteness, particle diameter, specific conductivity to it after crushing packing, 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 |
Shown 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%; Alumina 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 at 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, in enforcement process of the present invention, suitable experimental technique is used to help the public, obtain good experiment effect, this does not get rid of the equivalent experimental technique do not enumerated 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, distortion and amendment can also be applicable to.Should be understood that, the present invention includes all these distortion and amendment.Further, denomination of invention, title or similar part are to strengthen the public to understanding herein, should not being seen as limiting the scope of the present invention.
Make a general survey of whole specification sheets and claims, unless the context requires otherwise, otherwise word " comprises ", " comprising " and similar word, is interpreted as the implication that comprises and the implication of non-excluded, that is, looks like for " including, but are not limited to ".
Claims (20)
1. a preparation method for the coated barium sulfate of aluminium silicon, is characterized in that, comprise 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/L-0.15mol/L mixes, and obtains coated mixed solution;
(2) pre-treatment of barium sulfate: barium sulfate is pulled an oar according to the ratio that solid content is 20%-30%; Adding alkali adjusted to ph is afterwards 10 ~ 10.5, carries out emulsification afterwards and obtains barium sulfate emulsion; And
(3) coated finished product: barium sulfate emulsion step (2) obtained adds according to every cubic metre of molten emulsion of barium sulfate the ratio that 200-500 rises the coated mixed solution that step (1) obtains and mixes, and keeps the pH value of solution in mixing process more than 11; Carry out sealing steam-heated cal(l)andria afterwards; Stop heating cooling, by the pH regulator of cooled mixing solutions to 8.0-8.5, carry out solid-liquid separation afterwards, obtain solid and carry out washing, dry and obtain the coated barium sulfate product of aluminium silicon;
Wherein, described step (1) sodium aluminate prepares by the following method, metallic aluminium and sodium hydroxide reacted according to the ratio of Al=0.8mol/L-1.2mol/L, NaOH=1.2mol/L ~ 1.5mol/L, carry out solid-liquid separation after having reacted, obtain sodium aluminate liquid.
2. the preparation method of the coated barium sulfate of aluminium silicon according to claim 1, pulls an oar barium sulfate according to the ratio that solid content is 25% in wherein said step (2).
3. the preparation method of the coated barium sulfate of aluminium silicon according to claim 1, barium sulfate emulsion step (2) obtained in wherein said step (3) adds according to every cubic metre of molten emulsion of barium sulfate the ratio that 300-400 rises the coated mixed solution that step (1) obtains and mixes.
4. the preparation method of the coated barium sulfate of aluminium silicon according to any one of claim 1-3, 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 mixes.
5. the preparation method of the coated barium sulfate of aluminium silicon according to claim 4, wherein, reacts metallic aluminium and sodium hydroxide according to the ratio of Al=1.0mol/L, NaOH=1.3mol/L.
6. the preparation method of the coated barium sulfate of aluminium silicon according to claim 5, described step (1) is prepared temperature of reaction in sodium aluminate process and is controlled be less than or equal to 60 DEG C.
7. the preparation method of the coated barium sulfate of aluminium silicon according to claim 6, described step (1) is prepared temperature of reaction in sodium aluminate process and is controlled at 50 DEG C-60 DEG C.
8. the preparation method of the coated barium sulfate of aluminium silicon according to claim 7, described step (2) emulsification uses emulsification pump to carry out emulsification 1.5-3 hour.
9. the preparation method of the coated barium sulfate of aluminium silicon according to claim 1 or 8, the alkali that described step (2) adds is sodium hydroxide.
10. the preparation method of the coated barium sulfate of aluminium silicon according to claim 9, keeps the pH value of mixing solutions by adding sodium hydroxide in described step (3) mixing process.
11. according to claim 1 or 10 preparation method of the coated barium sulfate of aluminium silicon, the pH sulfuric acid of described step (3) cooled mixing solutions carries out being adjusted to 8.0-8.5.
12. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 11, and described step (3) heated sealed is warmed up to 105 DEG C of heating gradually in first 80 DEG C of heating.
13. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 12, and described step (3) heated sealed process is: intervally keep heating 1 hour at 80 ~ 85 DEG C, intervally keep heating 2 hours at 90 ~ 95 DEG C, in 100 ~ 105 DEG C of intervals, keep heating 1 hour.
14. according to claim 1 or 13 preparation method of the coated barium sulfate of aluminium silicon, described step (3) is cooled to and is less than 90 DEG C.
15., according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 14, carry out stirring 0.5-2 hour before described step (3) solid-liquid separation,
16. according to claim 1 or 15 preparation method of the coated barium sulfate of aluminium silicon, described step (3) washing is than for 1:(3-5 according to material quality) add water and carry out heat and wash, it is 80 ~ 90 DEG C that heat washes temperature, and described oven dry dries 5-7 hour at 140-160 DEG C.
17. according to the preparation method of the coated barium sulfate of aluminium silicon described in claim 16, and described oven dry is dried 6 hours at 150 DEG C.
18. 1 kinds of coated barium sulfate products of aluminium silicon prepared by preparation method described in any one of claim 1-17, its barium sulfate content is more than 95.00%; Alumina silicate content is within the scope of 1.00%-4.00%.
The coated barium sulfate product of 19. aluminium silicon as claimed in claim 18, its barium sulfate content is within the scope of 95.00-98.00%.
The coated barium sulfate product of 20. aluminium silicon as claimed in claim 18, its D
50between 0.200 micron-0.300 micron, whiteness is more than 98.5%, and specific conductivity is at below 70us/cm, and 325 mesh sieve residual values are less than 0.05%.
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| CN201410105069.0A CN103819937B (en) | 2014-03-20 | 2014-03-20 | Coated barium sulfate of a kind of aluminium silicon and preparation method thereof |
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| CN201410105069.0A CN103819937B (en) | 2014-03-20 | 2014-03-20 | Coated barium sulfate of a kind of aluminium silicon and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN86101534A (en) * | 1986-08-07 | 1988-02-17 | 上海京华化工厂 | The preparation method of water dispersing lide powder pigment |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE10026791A1 (en) * | 2000-05-31 | 2001-12-06 | Solvay Barium Strontium Gmbh | Micronized barium sulfate |
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Patent Citations (5)
| 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 |
| 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 |
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