CN110451549A - A kind of preparation method of high dispersive barite - Google Patents
A kind of preparation method of high dispersive barite Download PDFInfo
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- CN110451549A CN110451549A CN201910813195.4A CN201910813195A CN110451549A CN 110451549 A CN110451549 A CN 110451549A CN 201910813195 A CN201910813195 A CN 201910813195A CN 110451549 A CN110451549 A CN 110451549A
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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- C01F11/46—Sulfates
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Abstract
The invention discloses a kind of preparation methods of high dispersive barite, after barite coarse crushing, flour mill grinding are then added, obtains blanc fixe;Water and dispersing agent are added in blanc fixe, continues in ball mill grinding to partial size to be 20-200nm, filter, drying obtains nano barite;Reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:2-3, adds mixed acid, is stirred, and is filtered, washing;The mixed acid is made of citric acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid;The nano barite obtained after processing is delivered to surface modifying machine, and the surface treating agent of alkylnaphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane composition is added, stirs, and drying is broken up, and high dispersive blanc fixe is made.Barite powder made from this method not only increases dispersibility, moreover it is possible to improve the compatibility of powder and organic substrate, improve processing performance, the whiteness of product can reach 95%, widen the application of barite powder.
Description
Technical field
The present invention relates to technical field of inorganic material, the preparation method of specifically a kind of high dispersive barite.
Background technique
Barite be it is a kind of important containing baryta mineral, have the characteristics that big density, chemical property and thermal property stabilization.Mesh
Preceding barite deposit object is mainly applied in the low value-added field such as petrochemical industry, such as the chemical products of barite heavy weight additive, baric
Deng, and ultrafine barite powder is mainly used in coating, makes since granularity is fine, bigger serface, high chemical activity, Gao Baidu
The industrial departments such as paper, rubber, medicine;In recent years it also expands and is applied to the military projects high-tech area such as stealth material, radiation proof material.
The existing ultrafine barite powder for preparing commonly reaches micron order even Nano grade, since the partial size of powder is smaller
Can make it easier to reunite with high surface, dispersibility it is poor, reduce the mechanical property of material, secondly barite powder with it is organic
The compatibility of matrix is poor, to limit the application of ultrafine barite powder body.
Solve the problems, such as that ultrafine barite powder body bad dispersibility main means easy to reunite are carried out to barite powder at present
Surface is modified, and the surface treating agent of selection is usually fatty acid or its salt, although this method makes the dispersibility of powder obtain one
It is fixed to improve, but effect is unobvious, and is difficult to improve the consistency problem of powder and organic substrate.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept and technical solution of the invention, not
The prior art for necessarily belonging to present patent application shows above content in the applying date of present patent application in no tangible proof
In the case where having disclosed, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The present invention is in view of the deficienciess of the prior art, provide a kind of preparation method of high dispersive barite.Our legal system
Standby barite powder not only increases the dispersibility of powder, moreover it is possible to improve the compatibility of powder and organic substrate, improve processing
Performance, while the whiteness of product can reach 95%, widen the application of ultrafine barite powder body.
In order to achieve the goal above, The technical solution adopted by the invention is as follows:
A kind of preparation method of high dispersive barite, includes the following steps:
(1) after barite being crushed to 10-20 mesh, after then addition flour mill is ground to 400-800 mesh, barite is obtained
Powder;
(2) water is added in blanc fixe and dispersing agent is made into the suspension that mass concentration is 20-30%, continues in ball milling
It is 20-200nm that machine, which is ground to partial size, is filtered, and drying obtains nano barite;The dispersing agent is by polyethylene glycol stearate diester
It is formed with octyl phenol polyoxyethylene ether;
(3) reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:2-3, is heated to 50-60 DEG C, adds mixed
Acid is closed, stirs 20-30min, filtering, being washed to pH is 6-7;The mixed acid is sub- by citric acid, ethylenediamine tetra-acetic acid and hydroxyl
Ethyl di 2 ethylhexyl phosphonic acid composition;
(4) obtained nano barite after step (3) processing is delivered to surface modifying machine, be added alkylnaphthalene sulfonate and
The surface treating agent of trimethylsilyl cage type polysilsesquioxane composition, after stirring 30-60min, drying is broken up, and height is made
Disperse blanc fixe.
Further, the additional amount of step (2) described dispersing agent is the 1.5-2.5% of blanc fixe.
Further, the weight ratio of polyethylene glycol stearate diester and octyl phenol polyoxyethylene ether is 1- in the dispersing agent
3:1。
Further, the flour mill is vertical pulverizer.Preferably, vertical pulverizer be HLM vertical pulverizer or
HLMX super fine vertical flour mill.
Further, the additional amount of the mixed acid be citric acid 50-100g/L, ethylenediamine tetra-acetic acid 100-150g/L and
30-50g/L hydroxy ethylene diphosphonic acid.
Further, the additional amount of the surface treating agent is the 0.5-2% of blanc fixe weight.
Further: alkylnaphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane in the surface treating agent
Weight ratio be 2-4:1.
Compared with prior art, it advantages of the present invention and has the beneficial effect that
1, the present invention is added during grinding prepares nano barite by polyethylene glycol stearate diester and octylphenol polyethylene
The dispersing agent of ethylene oxide ether composition, can assign nano barite excellent oleophilic drainage performance, effectively increase point of powder
Property is dissipated, improves processing performance and stability, solves the problems, such as that ultrafine barite powder is easily reunited.
2, the present invention is additionally added alkylnaphthalene sulfonate and the surface of trimethylsilyl cage type polysilsesquioxane composition is living
Property agent blanc fixe is further modified, can effective strands such as absorbing fats acid, prevent the precipitation of dispersing agent, further mention
The dispersibility of high system, and trimethylsilyl cage type polysilsesquioxane is that one kind itself contains inorganic-organic mixed structure
Substance, the compatibility of blanc fixe Yu organic-inorganic substrate can be significantly improved, enable barite coating, papermaking,
The fields such as rubber are widely used.
3, the present invention is using the mixed acid of citric acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid composition using complexing
Reaction principle bleaches barite, and citric acid can dissolve the iron oxide in barite, and easily in impurity iron, calcium,
Complex reaction occurs for magnesium plasma, forms stable complex compound, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid can be to Ca2
+, the metal ions such as Mg2+, Cu2+, Fe2+ have good sequestering power so that the barite whiteness of preparation can reach 95%.And
The tart flavour organic acid that the present invention uses solves the problems, such as existing inorganic acid corrosion equipment to the corrosion-free phenomenon of equipment.
4, the present invention carries out grinding barite using HLM vertical pulverizer or HLMX super fine vertical flour mill, with ball mill
It compares, occupied area and energy consumption reduce 50% or so, and cost is relatively low, and it is easy to maintain, and PLC fully automatic system is used, automation
Degree is high.
5, the method for the present invention simple process, cost is relatively low, environment friendly and pollution-free, barite powder obtained can be applicable to top grade
The fields such as paint, coating, medical material, high-grade military project filler, are widely used, have good market prospects.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples;Also it is not construed as limitation of the present invention.
Embodiment 1
A kind of preparation method of high dispersive barite, includes the following steps:
(1) after barite being crushed to 20 mesh, after then addition HLM vertical pulverizer is ground to 500 mesh, barite is obtained
Powder;
(2) water is added in blanc fixe and dispersing agent is made into the suspension that mass concentration is 25%, continues in ball mill
Being ground to partial size is 150nm, is filtered, and drying obtains nano barite;The dispersing agent is that 2:1 polyethylene glycol is double hard by mass ratio
Resin acid ester and octyl phenol polyoxyethylene ether composition, additional amount are the 1.8% of blanc fixe weight;
(3) reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:2.5, is heated to 50 DEG C, adds by lemon
The mixed acid of acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid composition stirs 30min, and filtering, being washed to pH is 6.5;Institute
Stating mixed acid additional amount is citric acid 80g/L, ethylenediamine tetra-acetic acid 100g/L and 40g/L hydroxy ethylene diphosphonic acid;
(4) nano barite obtained after step (3) processing is delivered to surface modifying machine, it is 3:1's that weight ratio, which is added,
The surface treating agent of alkylnaphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane composition, the additional amount of surface treating agent
It is the 1.5% of blanc fixe weight, after stirring 60min, drying is broken up, and high dispersive blanc fixe product is made.
Using blanc fixe product made from YQ-Z-48A whiteness instrument the present embodiment, whiteness 95.24%.
Embodiment 2
A kind of preparation method of high dispersive barite, includes the following steps:
(1) after barite being crushed to 16 mesh, after then addition HLMX super fine vertical flour mill is ground to 600 mesh, weight is obtained
Spar powder;
(2) water is added in blanc fixe and dispersing agent is made into the suspension that mass concentration is 30%, continues in ball mill
Being ground to partial size is 80nm, is filtered, and drying obtains nano barite;The dispersing agent is that 1:1 polyethylene glycol is double stearic by mass ratio
Acid esters and octyl phenol polyoxyethylene ether composition, additional amount are the 2.2% of blanc fixe weight;
(3) reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:2, is heated to 60 DEG C, adds by lemon
The mixed acid of acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid composition stirs 25min, and filtering, being washed to pH is 7;It is described
Mixed acid additional amount is citric acid 100g/L, ethylenediamine tetra-acetic acid 120g/L and 35g/L hydroxy ethylene diphosphonic acid;
(4) nano barite obtained after step (3) processing is delivered to surface modifying machine, it is 2:1's that weight ratio, which is added,
The surface treating agent of alkylnaphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane composition, the additional amount of surface treating agent
It is the 0.8% of blanc fixe weight, after stirring 45min, drying is broken up, and high dispersive blanc fixe product is made.
Using blanc fixe product made from YQ-Z-48A whiteness instrument the present embodiment, whiteness 92.69%.
Embodiment 3
A kind of preparation method of high dispersive barite, includes the following steps:
(1) after barite being crushed to 10 mesh, after then addition HLMX super fine vertical flour mill is ground to 800 mesh, weight is obtained
Spar powder;
(2) water is added in blanc fixe and dispersing agent is made into the suspension that mass concentration is 30%, continues in ball mill
Being ground to partial size is 120nm, is filtered, and drying obtains nano barite;The dispersing agent is that 3:1 polyethylene glycol is double hard by mass ratio
Resin acid ester and octyl phenol polyoxyethylene ether composition, additional amount are the 1.5% of blanc fixe weight;
(3) reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:3, is heated to 55 DEG C, adds by lemon
The mixed acid of acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid composition stirs 30min, and filtering, being washed to pH is 6;It is described
Mixed acid additional amount is citric acid 70g/L, ethylenediamine tetra-acetic acid 150g/L and 30g/L hydroxy ethylene diphosphonic acid;
(4) nano barite obtained after step (3) processing is delivered to surface modifying machine, it is 4:1's that weight ratio, which is added,
The surface treating agent of alkylnaphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane composition, the additional amount of surface treating agent
It is the 1.0% of blanc fixe weight, after stirring 30min, drying is broken up, and high dispersive blanc fixe product is made.
Using blanc fixe product made from YQ-Z-48A whiteness instrument the present embodiment, whiteness 93.18%.
Embodiment 4
A kind of preparation method of high dispersive barite, includes the following steps:
(1) after barite being crushed to 20 mesh, after then addition HLM vertical pulverizer is ground to 400 mesh, barite is obtained
Powder;
(2) water is added in blanc fixe and dispersing agent is made into the suspension that mass concentration is 30%, continues in ball mill
Being ground to partial size is 50nm, is filtered, and drying obtains nano barite;The dispersing agent is that 2:1 polyethylene glycol is double stearic by mass ratio
Acid esters and octyl phenol polyoxyethylene ether composition, additional amount are the 1.5% of blanc fixe weight;
(3) reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:2.5, is heated to 60 DEG C, adds by lemon
The mixed acid of acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphonic acid composition stirs 25min, and filtering, being washed to pH is 7;It is described
Mixed acid additional amount is citric acid 100g/L, ethylenediamine tetra-acetic acid 120g/L and 35g/L hydroxy ethylene diphosphonic acid;
(4) nano barite obtained after step (3) processing is delivered to surface modifying machine, it is 2:1's that weight ratio, which is added,
The surface treating agent of alkylnaphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane composition, the additional amount of surface treating agent
It is the 1.2% of blanc fixe weight, after stirring 60min, drying is broken up, and high dispersive blanc fixe product is made.
Using blanc fixe product made from YQ-Z-48A whiteness instrument the present embodiment, whiteness 91.28%.
Using Patent No. 201610089788.7, patent name is corrosion resistant epoxy novolac coating under insulating layer, real
The formula and method for applying example 1 prepare coating, and the product of embodiment 1-4 is respectively adopted in the barite in formula, conventionally
The performance of coating is measured, test result is as shown in table 1.
Table 1: barite powder produced by the present invention applies the performance test results in epoxy novolac coating
It is learnt from above-mentioned test result, blanc fixe produced by the present invention, which is applied, to be applied in epoxy novolac coating, coating
Adhesive force significantly improve, illustrate that barite produced by the present invention and other coating substrates have good compatibility.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot
Assert that specific implementation of the invention is only limited to these instructions.General technical staff of the technical field of the invention is come
It says, without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described,
And these substitutions or variant are regarded as belonging to the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of high dispersive barite, characterized by the following steps:
After barite is crushed to 10-20 mesh, after then addition flour mill is ground to 400-800 mesh, blanc fixe is obtained;
Water and dispersing agent are added in blanc fixe and is made into the suspension that mass concentration is 20-30%, continue ball mill grinding extremely
Partial size is 20-200nm, is filtered, and drying obtains nano barite;The dispersing agent is by polyethylene glycol stearate diester and octyl phenol
Polyoxyethylene ether composition;
Reaction kettle is added in nano barite, adding water to solid-to-liquid ratio is 1:2-3, is heated to 50-60 DEG C, adds mixed acid, stirs
20-30min is mixed, is filtered, being washed to pH is 6-7;The mixed acid is by citric acid, ethylenediamine tetra-acetic acid and hydroxy ethylene diphosphine
Acid composition;
The nano barite obtained after step (3) processing is delivered to surface modifying machine, alkylnaphthalene sulfonate and trimethyl is added
The surface treating agent of silylation cage type polysilsesquioxane composition, after stirring 30-60min, drying is broken up, and high score bulk weight is made
Spar powder.
2. the preparation method of high dispersive barite according to claim 1, it is characterised in that: step (2) described dispersing agent
Additional amount is the 1.5-2.5% of blanc fixe.
3. the preparation method of high dispersive barite according to claim 2, it is characterised in that: polyethylene glycol in the dispersing agent
The weight ratio of double stearates and octyl phenol polyoxyethylene ether is 1-3:1.
4. the preparation method of high dispersive barite according to claim 1, it is characterised in that: the flour mill is vertical milling
Machine.
5. the preparation method of high dispersive barite according to claim 4, it is characterised in that: the vertical pulverizer is HLM
Vertical pulverizer or HLMX super fine vertical flour mill.
6. the preparation method of high dispersive barite according to claim 1, it is characterised in that: the additional amount of the mixed acid is
Citric acid 50-100g/L, ethylenediamine tetra-acetic acid 100-150g/L and 30-50g/L hydroxy ethylene diphosphonic acid.
7. the preparation method of high dispersive barite according to claim 1, it is characterised in that: the addition of the surface treating agent
Amount is the 0.5-2% of blanc fixe weight.
8. the preparation method of high dispersive barite according to claim 7, it is characterised in that: alkyl in the surface treating agent
The weight ratio of naphthalene sulfonate and trimethylsilyl cage type polysilsesquioxane is 2-4:1.
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CN114314631A (en) * | 2022-01-21 | 2022-04-12 | 贵州理工学院 | Treatment method for purifying and whitening barite |
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