CN102167386A - Method for preparing barium sulfate nanoparticles - Google Patents
Method for preparing barium sulfate nanoparticles Download PDFInfo
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- CN102167386A CN102167386A CN 201110063603 CN201110063603A CN102167386A CN 102167386 A CN102167386 A CN 102167386A CN 201110063603 CN201110063603 CN 201110063603 CN 201110063603 A CN201110063603 A CN 201110063603A CN 102167386 A CN102167386 A CN 102167386A
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- barium
- solution
- suspension liquid
- metabisulfite solution
- barium sulfate
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Abstract
The invention discloses a method for preparing barium sulfate nanoparticles, belonging to the technical field of preparation of chemical materials. The method comprises the following steps: vertically dispersing a sodium sulfate solution into a flowing barium sulphide solution or circularly following barium sulphide suspension liquid through a plurality of micropores, cutting the sodium sulfate solution by means of cross flow, reacting in a mixing way to obtain a barium sulfate precipitate, and carrying out curing, solid-liquid separation, impurity removal in a washing way, drying and smashing on reaction product to obtain the barium sulfate nanoparticles. The method for preparing the barium sulfate nanoparticles is low in raw material cost, high in production capacity, simple and convenient in operation process, and good in repeatability and stability, so that the conventional mirabilite-black ash method can enter into the production sequence of the nanometer level barium sulfate nanoparticles. The method can be used for preparing the barium sulfate nanoparticles with the mean grain sizes of 35-48nm.
Description
Technical field
The invention belongs to technical field of chemical material preparation, particularly a kind of preparation barium sulphate nano particulate method specifically, relates to a kind of micropore dispersion method of utilizing the liquid phase cross-flow to shear and prepares barium sulphate nano particulate method.
Background technology
The barium sulphate nano particle has small-size effect and good chemical stability, is widely used in fields such as the packing material of coating, plastics, paint and additive.Barium sulphate nano preparation method of granules at present commonly used mainly contains: (1) saltcake-grey black method-with sodium sulphite, barium bittern and sodium sulfate is a raw material, at first obtain barium sulfide solution or slurry, mix with metabisulfite solution afterwards, chemical reaction takes place, regulate the pH value afterwards to reaction end, obtain the barium sulfate slurry, and finally obtain product; (2) complexing-precipitator method-with BaCl
2With EDTA solution be raw material, with the two mixed preparing Ba
2+The complex system of-EDTA is regulated complex system and is reached certain pH value and temperature; The Na that will prepare in advance then
2SO
4React in the solution adding complex system, reaction product promptly gets the nano barium sulfate product through centrifugation, washing, drying.These methods or introduce other reactive component strengthen the later separation difficulty; Prepare perhaps that gained particulate granularity is bigger than normal, wider distribution, monodispersity be not good, as saltcake-grey black method, the existing particle diameter of this handicraft product is difficult to reach nano level.It is poor that the reason that produces this situation is that the material microcosmic mixes, and transmittance process is slow, and the nucleation amount is little when directly precipitating, nucleation is inhomogeneous, and has directly influenced the particulate quality.
On the other hand, utilize the micropore of fluid shearing to disperse good performance is all arranged for homogeneous phase and heterogeneous mixing, system heat and mass efficient height, help to solve rapid reaction because of transmitting the problem of restriction poor controllability, for direct precipitation method has been created condition making a breakthrough aspect the preparation barium sulphate nano particle.
Summary of the invention
The present invention is intended to propose a kind of new preparation barium sulphate nano particulate method.Its principle is: what selected system took place among the present invention is the liquid-phase precipitation reaction, and speed of response is fast, and transmittance process is the controlled step in the preparation process; For this system, utilize the micropore of fluid shearing to disperse to accelerate the carrying out of transmitting, making has higher degree of supersaturation in the system, guaranteed the blended homogeneity simultaneously, thereby prepares the barium sulphate nano particle that particle is little and be evenly distributed.
A kind of preparation barium sulphate nano particulate method, with metabisulfite solution from vertical direction be distributed to the mobile barium sulfide solution by micropore or the barium sulphide suspension liquid that circulates, metabisulfite solution is sheared by cross-flow, hybrid reaction, generate barium sulfate precipitate, reaction product makes the barium sulphate nano particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing.
The temperature of described barium sulfide solution or suspension liquid is 10～70 ℃, and the temperature of described metabisulfite solution is 10～70 ℃.
The concentration of described barium sulfide solution or suspension liquid is 0.25～2.5mol/L, and the concentration of described metabisulfite solution is 5～45wt%.
Described micropore equivalent diameter is 0.2～1000 micron.
The flow velocity of barium sulfide solution or suspension liquid is 0.2～3m/s, and the flow velocity of metabisulfite solution is 0.1～5m/s.
Specifically, the method for the invention comprises the steps:
(1) formulating vulcanization barium solution or barium sulphide suspension liquid;
(2) preparation metabisulfite solution;
(3) under pressure, make metabisulfite solution from vertical direction be distributed to the mobile barium sulfide solution by micropore or the barium sulphide suspension liquid that circulates, metabisulfite solution is sheared by cross-flow, hybrid reaction;
(4) reaction product obtains final barium sulphate nano particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing (press industrial standards and pulverize, be i.e. 45 μ m screenings content≤0.5%).
In the step (3), the molar flow rate of the molar flow rate of the sodium sulfate of bringing into metabisulfite solution and the barium sulphide brought into barium sulfide solution equates.
In the step (3), the barium sulphide suspension liquid constantly circulates, and barium sulphide molar weight initial in the molar weight of the sodium sulfate of bringing into metabisulfite solution and barium sulphide suspension liquid equates.
Beneficial effect of the present invention is: utilize method of the present invention to prepare the barium sulphate nano particle, raw materials cost is low, and throughput is big, and operating process is easy, repeatability and good stability make traditional saltcake-grey black method can enter the production sequence of nano level barium sulfate particle.Adopt this method can obtain the barium sulphate nano particle of median size at 35～48nm.
Embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1:
Under 70 ℃, preparation 1000mL volumetric molar concentration is that the barium sulphide suspension liquid of 2.5mol/L and 800g massfraction are 45% metabisulfite solution.Under the effect of pressure reduction, it is that 200 microns micropore mixes with the barium sulphide suspension liquid that circulates do cross-flow, flow velocity is 1m/s that metabisulfite solution passes equivalent diameter with the flow velocity of 0.5m/s, and reaction generates barium sulfate precipitate, and circulating reaction is to stoicheiometry.Product obtains final barium sulfate particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing, and its median size is 48nm.
Embodiment 2:
Under 50 ℃, preparation 1000mL volumetric molar concentration is that the barium sulfide solution of 1.5mol/L and 720g massfraction are 30% metabisulfite solution.Under the effect of pressure reduction, it is that 200 microns micropore is that the barium sulfide solution of 3m/s mixes with making cross-flow passes, flow velocity that metabisulfite solution passes equivalent diameter with the flow velocity of 5m/s, and reaction generates barium sulfate precipitate.Product obtains final barium sulfate particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing, and its median size is 43nm.
Embodiment 3:
Under 20 ℃, preparation 1000mL volumetric molar concentration is that the barium sulphide suspension liquid of 0.5mol/L and 720g massfraction are 10% metabisulfite solution.Under the effect of pressure reduction, it is that 600 microns micropore mixes with the barium sulphide suspension liquid that circulates do cross-flow, flow velocity is 0.3m/s that metabisulfite solution passes equivalent diameter with the flow velocity of 0.1m/s, and reaction generates barium sulfate precipitate, and circulating reaction is to stoicheiometry.Product obtains final barium sulfate particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing, and its median size is 40nm.
Embodiment 4:
Under 10 ℃, preparation 1000mL volumetric molar concentration is that the barium sulfide solution of 0.25mol/L and 720g massfraction are 5% metabisulfite solution.Under the effect of pressure reduction, it is that 0.2 micron micropore is that the barium sulfide solution of 0.2m/s mixes with making cross-flow passes, flow velocity that metabisulfite solution passes equivalent diameter with the flow velocity of 0.2m/s, and reaction generates barium sulfate precipitate.Product obtains final barium sulfate particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing, and its median size is 35nm.
Embodiment 5:
Under 40 ℃, preparation 1000mL volumetric molar concentration is that the barium sulfide solution of 1.0mol/L and 720g massfraction are 20% metabisulfite solution.Under the effect of pressure reduction, it is that 200 microns micropore is that the barium sulfide solution of 1m/s mixes with making cross-flow passes, flow velocity that metabisulfite solution passes equivalent diameter with the flow velocity of 0.5m/s, and reaction generates barium sulfate precipitate.Product obtains final barium sulfate particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing, and its median size is 37nm.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (9)
1. one kind prepares barium sulphate nano particulate method, it is characterized in that: with metabisulfite solution from vertical direction be distributed to the mobile barium sulfide solution by micropore or the barium sulphide suspension liquid that circulates, metabisulfite solution is sheared by cross-flow, hybrid reaction, generate barium sulfate precipitate, reaction product makes the barium sulphate nano particle through aftertreatment.
2. method according to claim 1 is characterized in that: described aftertreatment comprises the steps: slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing.
3. method according to claim 1 is characterized in that: the temperature of described barium sulfide solution or suspension liquid is 10～70 ℃, and the temperature of described metabisulfite solution is 10～70 ℃.
4. method according to claim 1 is characterized in that: the concentration of described barium sulfide solution or suspension liquid is 0.25～2.5mol/L, and the concentration of described metabisulfite solution is 5～45wt%.
5. method according to claim 1 is characterized in that: described micropore equivalent diameter is 0.2～1000 micron.
6. method according to claim 1 is characterized in that: the flow velocity of barium sulfide solution or suspension liquid is 0.2～3m/s, and the flow velocity of metabisulfite solution is 0.1～5m/s.
7. method according to claim 1 is characterized in that comprising the steps:
(1) formulating vulcanization barium solution or barium sulphide suspension liquid;
(2) preparation metabisulfite solution;
(3) under pressure, make metabisulfite solution from vertical direction be distributed to the mobile barium sulfide solution by micropore or the barium sulphide suspension liquid that circulates, metabisulfite solution is sheared by cross-flow, hybrid reaction;
(4) reaction product obtains the barium sulphate nano particle through slaking, solid-liquid separation, washing removal of impurities, drying, pulverizing.
8. method according to claim 7 is characterized in that: in the step (3), the molar flow rate of the molar flow rate of the sodium sulfate of bringing into metabisulfite solution and the barium sulphide brought into barium sulfide solution equates.
9. method according to claim 7 is characterized in that: in the step (3), the barium sulphide suspension liquid constantly circulates, and barium sulphide molar weight initial in the molar weight of the sodium sulfate of bringing into metabisulfite solution and barium sulphide suspension liquid equates.
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| CN 201110063603 CN102167386B (en) | 2011-03-16 | 2011-03-16 | Method for preparing barium sulfate nanoparticles |
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|---|---|---|---|
| CN 201110063603 CN102167386B (en) | 2011-03-16 | 2011-03-16 | Method for preparing barium sulfate nanoparticles |
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| CN102167386B CN102167386B (en) | 2013-07-03 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130260A (en) * | 2013-03-19 | 2013-06-05 | 冉金友 | Production method of barium sulfate |
| CN104512923A (en) * | 2013-09-30 | 2015-04-15 | 上海梅山钢铁股份有限公司 | Preparation method of nano-barium sulfate |
| CN106241850A (en) * | 2016-07-12 | 2016-12-21 | 重庆工商大学 | The preparation method and applications of insoluble sulfur hydrochlorate photocatalyst |
| CN106745152A (en) * | 2015-11-25 | 2017-05-31 | 宜宾丝丽雅股份有限公司 | A kind of method for preparing nano barium sulfate and co-producing sodium chloride |
| CN111285389A (en) * | 2018-12-06 | 2020-06-16 | 南风化工集团股份有限公司 | Production method of superfine precipitated barium sulfate |
| CN111362293A (en) * | 2020-04-03 | 2020-07-03 | 河北化工医药职业技术学院 | Preparation method of spindle-shaped barium sulfate and spindle-shaped barium sulfate |
| CN111533153A (en) * | 2020-04-20 | 2020-08-14 | 中国日用化学研究院有限公司 | Preparation method of nano barium sulfate powder |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377831A (en) * | 2001-04-03 | 2002-11-06 | 黄榕 | Process for preparing super fine deposited barium sulphate |
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
| CN101423239A (en) * | 2008-11-21 | 2009-05-06 | 北京化工大学 | Method for preparing nano barium sulfate with controllable particle size distribution |
| CN101580262A (en) * | 2009-04-08 | 2009-11-18 | 王嘉兴 | Method for preparing nano barium sulphate series products by using barium slag |
| CN101798090A (en) * | 2010-04-07 | 2010-08-11 | 清华大学 | Method for preparing nanometer silicon dioxide |
| CN101811685A (en) * | 2010-04-07 | 2010-08-25 | 清华大学 | Method for preparing beta-calcium phosphate or hydroxyapatite nanoparticles |
| CN101823752A (en) * | 2009-04-13 | 2010-09-08 | 王嘉兴 | Method for co-production of hydrochloric acid in preparation of nano barium sulfate by barium chloride |
-
2011
- 2011-03-16 CN CN 201110063603 patent/CN102167386B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377831A (en) * | 2001-04-03 | 2002-11-06 | 黄榕 | Process for preparing super fine deposited barium sulphate |
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
| CN101423239A (en) * | 2008-11-21 | 2009-05-06 | 北京化工大学 | Method for preparing nano barium sulfate with controllable particle size distribution |
| CN101580262A (en) * | 2009-04-08 | 2009-11-18 | 王嘉兴 | Method for preparing nano barium sulphate series products by using barium slag |
| CN101823752A (en) * | 2009-04-13 | 2010-09-08 | 王嘉兴 | Method for co-production of hydrochloric acid in preparation of nano barium sulfate by barium chloride |
| CN101798090A (en) * | 2010-04-07 | 2010-08-11 | 清华大学 | Method for preparing nanometer silicon dioxide |
| CN101811685A (en) * | 2010-04-07 | 2010-08-25 | 清华大学 | Method for preparing beta-calcium phosphate or hydroxyapatite nanoparticles |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130260A (en) * | 2013-03-19 | 2013-06-05 | 冉金友 | Production method of barium sulfate |
| CN103130260B (en) * | 2013-03-19 | 2014-11-19 | 冉金友 | Production method of barium sulfate |
| CN104512923A (en) * | 2013-09-30 | 2015-04-15 | 上海梅山钢铁股份有限公司 | Preparation method of nano-barium sulfate |
| CN106745152A (en) * | 2015-11-25 | 2017-05-31 | 宜宾丝丽雅股份有限公司 | A kind of method for preparing nano barium sulfate and co-producing sodium chloride |
| CN106241850A (en) * | 2016-07-12 | 2016-12-21 | 重庆工商大学 | The preparation method and applications of insoluble sulfur hydrochlorate photocatalyst |
| CN106241850B (en) * | 2016-07-12 | 2018-01-02 | 重庆工商大学 | The preparation method and applications of insoluble sulfur hydrochlorate photochemical catalyst |
| CN111285389A (en) * | 2018-12-06 | 2020-06-16 | 南风化工集团股份有限公司 | Production method of superfine precipitated barium sulfate |
| CN111362293A (en) * | 2020-04-03 | 2020-07-03 | 河北化工医药职业技术学院 | Preparation method of spindle-shaped barium sulfate and spindle-shaped barium sulfate |
| CN111533153A (en) * | 2020-04-20 | 2020-08-14 | 中国日用化学研究院有限公司 | Preparation method of nano barium sulfate powder |
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| CN102167386B (en) | 2013-07-03 |
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