CN101423239A - Method for preparing nano barium sulfate with controllable particle size distribution - Google Patents

Method for preparing nano barium sulfate with controllable particle size distribution Download PDF

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Publication number
CN101423239A
CN101423239A CNA2008102267384A CN200810226738A CN101423239A CN 101423239 A CN101423239 A CN 101423239A CN A2008102267384 A CNA2008102267384 A CN A2008102267384A CN 200810226738 A CN200810226738 A CN 200810226738A CN 101423239 A CN101423239 A CN 101423239A
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particle size
baso
reactor
preparation
size distribution
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CNA2008102267384A
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李殿卿
郭盛昌
林彦军
徐向宇
段雪
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

The invention provides a preparation method of nano barium sulfate with the controllable particle size distribution. The preparation method takes BaCl2 and Na2SO4 as raw materials, respectively prepares two types of solution and then simultaneously adds the two types of solution into a rotary liquid membrane reactor with the high-speed rotation at the same flow rate for carrying out nucleation reaction, and centrifugal washing and drying are carried out to the obtained slurry to obtain the nano BaSO4 with the particle size of 30-120nm and the narrower particle size distribution. The purpose of precisely controlling the particle size of the product can be achieved by regulating and controlling the rotational speed, the gap and other operation parameters of the reactor, thereby being capable of preparing the BaSO4 with the particle size of 30-40nm. The method combines the advantages of a micro-reactor and a high gravity reactor and simultaneously avoids the shortcomings of the micro-emulsion method, the complex method and the like, thereby having small reaction space and high preparation speed and being capable of meeting the requirements on the industrial preparation of the nano BaSO4.

Description

A kind of method for preparing nano barium sulfate of controllable particle size distribution
Technical field:
The present invention relates to the preparation field of inorganic non-metallic functional materials, be specifically related to a kind of nanometer BaSO of controllable particle size distribution 4The preparation method.
Technical background:
BaSO 4Being a kind of unbodied white powder, belonging to rhombic system, is the very stable inorganic salt of a kind of chemical property, and with any material generation chemical reaction, whiteness is very high, can absorb harm ray hardly, and proportion is the material of proportion maximum in all inorganic salt.Be widely used in industries such as oil drilling, plastics, rubber, coating, medium-to-high grade printing ink, medicine are synthetic, chemical industry, pigment, papermaking, pottery, makeup owing to its excellent physical chemistry.At present, BaSO 4Development trend be to improve value-added content of product such as surface modification and fine particlesization etc., to satisfy different specific demands.
Preparation nanometer BaSO 4Method mainly contain microemulsion method, complexometry, microreactor method, overweight force method and other preparation method.The prepared BaSO of microemulsion method and complexometry 4Have shortcomings such as foreign matter content is higher, aftertreatment complexity.The microreactor method is because the reactor size restriction is difficult to large-scale industrial production.Though overweight force method output is big, efficient is high, prepared size distribution broad, the degree that becomes more meticulous is not enough.Some other preparation method such as physical vapor deposition (PVD) method, chemical gaseous phase deposition (CVD) method, plasma body spray method etc. are because preparation condition limits, and speed of response is slower, and cost is higher, also is not suitable for industrial applications.Therefore, develop more and more important that a kind of production efficiency height, product purity height, particle diameter are little, the production technique of narrow diameter distribution becomes.
Microemulsion method is with BaCl 2And Na 2SO 4Solution is mixed with corresponding w/o type microemulsion system respectively, because the mutual exchange or the transmission of material in the water nuclear have taken place in collision mutually between the microemulsion micelle particle, causes the chemical reaction in the nuclear.Because the water nuclear radius is fixed, make reaction nucleation and growth only be limited in the fixed water nuclear, so therein the size of particles of Sheng Chenging also must control.This shows that the size of water nuclear has been controlled the particle diameter of nanoparticle, thereby influence the size that the big or small factor of micro emulsion micelle water nuclear will influence the nanoparticle of reaction generation.The nanometer BaSO that this method is prepared 4Contain organic impurities, purity is not high, also needs further aftertreatment.Document: XinyuSong, Sixiu Sun, Weiliu Fan, Zhilei Yin, Self-assemblies of the different morphologyultrafine barium sulfate in situ interface, Materials Letters 57 (2003) 3026-3030 have reported SO 4 2-Be attached on the organic amine, forming an end is polar SO 4 2-, making that an end is nonpolar long chain alkane, reaction formula is as follows:
2R 1R 2CHNH 2+H 2SO 4＝R 1R 2CHNH) 2SO 4
With heptane as non-polar solvent, Ba 2+The aqueous solution is polar solvent, makes emulsion, Ba 2+And SO 4 2-In the formed small micelle of organosulfur acid amide precipitin reaction takes place, making median size is the spherical BaSO of 20-30nm 4Crystal.Contain organic substances such as organic amine and heptane in the preparation process, degree of purity of production is had very big influence.
Complexometry is with BaCl 2Be hybridly prepared into Ba with EDTA solution 2+The complex system of-EDTA, the Na that will prepare in advance then 2SO 4Solution is poured in the complex system and is reacted, and reaction product gets nanometer BaSO through centrifugation, washing, drying 4Product.Document: Liu Youzhi, Li Junping, you win the member, Liu Laishuan, BaSO 4Nanoparticle preparation method research, application foundation and engineering science journal, 2001 Vol.9 No.2 P141-145 have reported with EDTA to be that complexing agent prepares nanometer BaSO 4Method, the BaSO of gained 4Median size is 47nm.This method can be introduced EDTA impurity, brings certain difficulty to aftertreatment.
The microreactor method is to utilize tiny Y type of reaction compartment or T type microreactor, prepares nanometer BaSO 4Reach microcosmic blended effect by the reaction compartment yardstick that reduces reactor, the reaction compartment of microreactor is generally several millimeters.Document: N.Kockmann, J.Kastner and P.Woias, Reactive particle precipitation inliquid microchannel flow, Chemical Engineering Journal, Volume 135, and Supplement 1,15January 2008, Pages S110-S116 has reported and has utilized T type reactor, and preparing the particle median size in ethanol-water solution system is the spherical BaSO of 20-70nm 4Crystal.The microreactor method is difficult to carry out heavy industrialization and uses because the reactor monolith structure is too small.
Overweight force method is to utilize parts such as wire packing generation strong wallop, shearing force, the frictional force of high speed rotating to cause the intensive field of turbulent flow, thereby make BaSO in supergravity reactor 4Particle is pulverized and is diminished.Document: you win the member, Liu Youzhi, Li Junping, Liu Laishuan, BaSO 4The liquid-phase synthesis process of nano-powder, the chemical engineer, Sum 86No15,2001, reported that the usefulness hypergravity is rotary packed bed as conversion unit, with BaCl 2And Na 2SO 4Solution is raw material, and the preparation median size is the nanometer BaSO of 80nm 4Overweight force method is bigger owing to the reaction compartment yardstick, thereby causes BaSO 4The crystal particle diameter wider distribution.
Summary of the invention:
The nanometer BaSO that the purpose of this invention is to provide a kind of controllable particle size distribution 4The preparation method.
The present invention is carried out to nuclear reaction with barium salt solution and sulfate liquor in the full back-mixing liquid film reactor of adding high speed rotating, obtains comparatively pure nano BaSO 4Precipitation.Operating parameterss such as the rotating speed by full back-mixing liquid film reactor in the conditioned reaction process, gap reach the purpose of accurate control product particle diameter.This method combines the advantage of microreactor and supergravity reactor, and reaction compartment is little, and preparation speed is fast, and the high speed rotating effect owing to the inside reactor rotor simultaneously forms powerful shearing force field, the BaSO that can make generation 4Carry out fast rotational, carry out high-intensity rubbing effect between particle, thereby stop nucleus further to be grown up.
Full back-mixing liquid film reactor is that ZL00132145.5 is seen for the novel reaction equipment that the through engineering approaches research of carrying out the nanometer laminated structure functional materials designs in this laboratory.The present invention is according to preparation BaSO 4Arts demand with the speed range of rotor for being set in 1000-5000rpm.Outside stator maintains static, and the gap adjustment range between rotor and the stator is adjusted into 0.1-0.5mm.The basic functional principle of full back-mixing liquid film reactor is to shear, grind and the high-speed stirring effect, it is anti-to strengthen three biographies one, relies on the relative movement of two conical surfaces, make by the material between the slit and be subjected to great shearing force and frictional force, thereby reach the effect of quick microcosmic hybrid reaction.
BaSO of the present invention 4Concrete preparation method as follows:
A. the soluble barium salt is dissolved in that compound concentration is the barium salt solution of 0.01-1.3M in the deionized water; Soluble sulphate or sulfuric acid are dissolved in the deionized water, and compound concentration is vitriol or the sulphuric acid soln of 0.01-1.3M;
Used soluble barium salt is BaCl 22H 2O, BaS, Ba (NO 3) 2Or BaCl 2, purity is analytical pure; Used soluble sulphate is Na 2SO 4, MgSO 4, ZnSO 4Or AlSO 4, purity is analytical pure; Used sulfuric acid is 98% the vitriol oil; The electric conductivity of used deionized water is not more than 10 -6S/cm; Because the contained impurity of reactive system can influence nucleation, cause crystal particle diameter excessive;
B. the gap width of adjusting between full back-mixing liquid film reactor rotor and the stator is 0.1-0.5mm, rotating speed is 1000-5000rpm, after the question response device stabilization of speed, with the feed rate of 150-620ml/min mol ratio barium salt solution and vitriol or sulphuric acid soln are added in the full back-mixing liquid film reactor, be carried out to nuclear reaction by 1:1; Because BaSO 4Content long-pending very little, reaction moment can finish; Keep being connected with in the outer stator chuck 25 ℃ water of condensation in the reaction process, after each reaction finishes,, remain in BaSO in the reactor to remove preparation process last time with the full back-mixing liquid film reactor of washed with de-ionized water inwall 4
C. collect suspension slurry from reactor outlet, filter, exist with deionized water centrifuge washing to aqueous phase inclusion-free ion, the gained filter cake was placed the 60-80 ℃ of dry 10-15 of baking oven hour, obtaining median size is 30-120nm nanometer BaSO 4
By the condition of regulation and control step B, can control prepared BaSO 4Particle diameter, promptly in the condition and range that step B is given, the rotating speed of rotor is high more, big more, the prepared BaSO in gap between rotor and the stator 4Median size is just more little; When the rotating speed of rotor is gap between 4000-5000rpm, rotor and the stator when being 0.4-0.5mm, the BaSO of preparation 4Median size is stabilized in about 30-40nm.
Because the full back-mixing liquid film reactor that is adopted is an industrial equipment, so the present invention can realize suitability for industrialized production.
Analyze BaSO with Shimadzu XRD-6000 type X-ray diffractometer 4The crystalline structure of sample (Cu target, K α source of radiation, λ are 0.15406nm, 5 °/min of sweep velocity, 20～60 ° of sweep limits).
By HITACHI H-800 type transmission electron microscope (acceleration voltage is 200kv) observing samples crystal morphology.
As shown in Figure 1, a is that full back-mixing liquid film reactor is at the nanometer BaSO of feed rate for preparation 4The XRD spectra of sample, b is the prepared big particle diameter BaSO of common stirred tank reactor 4BaSO has appearred in the XRD spectra of sample among the figure 4Characteristic diffraction peak, each main diffraction peak position is consistent with standard spectrogram JCPDS no.24-1035, does not have the appearance at other dephasign peak, illustrates that the synthetic sample is comparatively purified BaSO 4Crystal.Compare with common stirred tank reactor, with the BaSO of full back-mixing liquid film reactor preparation 4Each diffraction peak a little less than, peak shape is low flat, the peak width at half height broad, wherein (311) and (212) two diffraction peaks merge, this illustrates that full back-mixing liquid film reactor is to BaSO 4Nucleation and crystal structure produced influence, changed BaSO 4The crystal face pattern.According to the Xie Er formula, its more weak peak peak width at half height strong and broad illustrates that also formed crystal particle diameter is less.
As shown in Figure 2, the transmission electron microscope(TEM) phenetic analysis is the result show, the BaSO of the present invention's preparation 4The crystal median size can regulate and control between the 30-120nm, size distribution is also narrower.
The present invention has adopted full back-mixing liquid film reactor to prepare nanometer BaSO first 4Precipitation, major advantage are can prepare nano level BaSO on less reaction compartment yardstick under the prerequisite that guarantees production efficiency 4Crystal, products therefrom purity is higher, and crystal particle diameter is less, and narrow distribution can realize suitability for industrialized production nanometer BaSO 4
Description of drawings:
Fig. 1 is BaSO 4XRD spectra
Wherein a is embodiment 1 gained nanometer BaSO 4XRD spectra; B is the BaSO of common stirred tank reactor preparation 4XRD spectra.
Fig. 2 is the BaSO of preparation 4The TEM photo
Wherein a is the BaSO of embodiment 1 gained 4The TEM photo, b is the BaSO of embodiment 3 gained 4The TEM photo, c is the BaSO of embodiment 5 gained 4The TEM photo, d is the BaSO of embodiment 10 gained 4The TEM photo.
Embodiment:
Embodiment 1:
Steps A: take by weighing 317g BaCl 22H 2The Na of O and 218g 2SO 4, be dissolved in the deionized water, being made into concentration respectively is 1.3M, volume is the solution of 1L.
Step B: the gap width of adjusting full back-mixing liquid film reactor is 0.3mm, and rotating speed is 1000rpm, with the feed rate of 210ml/min two kinds of solution is added in the full back-mixing liquid film reactor simultaneously, is carried out to nuclear reaction.
Step C: collect suspension slurry and do not have Cl with deionized water centrifuge washing to aqueous phase from reactor outlet -Exist.Place 70 ℃ of baking ovens to obtain nanometer BaSO in dry 12 hours the gained filter cake 4
Prepared BaSO 4Characterize through TEM, see Fig. 2 a, recording median size is 120nm.
Embodiment 2:
Steps A: the Ba (NO that takes by weighing 8.5g 3) 2, be dissolved in that to be configured to concentration in the deionized water be that 0.0425M, volume are the solution of 1L, measure 4.25g concentration and be 98% the vitriol oil, be dissolved in the deionized water, be configured to concentration 0.0425M, volume is the sulphuric acid soln of 1L.
Step B: the gap width of adjusting full back-mixing liquid film reactor is 0.3mm, and rotating speed is 1000rpm, with the speed of 210ml/min two kinds of solution is added in the full back-mixing liquid film reactor simultaneously, is carried out to nuclear reaction.
Step C: collect suspension slurry and use the deionized water centrifuge washing to PH=7 from reactor outlet.Place 60 ℃ of baking ovens to obtain nanometer BaSO in dry 14 hours the gained filter cake 4
Prepared BaSO 4Characterize through TEM, recording median size is 80nm.
Embodiment 3:
Keep other preparation condition constant in embodiment 1, in step B the reactor rotating speed is adjusted into 2000rpm, the feed rate of peristaltic pump is increased to 250ml/min.The BaSO that finally obtains 4Characterize through TEM, see Fig. 2 b, recording median size is 61nm.
Embodiment 4:
Keep other preparation condition constant in embodiment 1, in step B the reactor rotating speed is adjusted into 3000rpm, the feed rate of peristaltic pump is increased to 400ml/min.The BaSO that finally obtains 4Median size is 43nm.
Embodiment 5:
Keep other preparation condition constant in embodiment 1, in step B the reactor rotating speed is adjusted into 4000rpm, the feed rate of peristaltic pump is increased to 480ml/min.The BaSO that finally obtains 4Characterize through TEM, see Fig. 2 c, recording median size is 35nm.
Embodiment 6:
Keep other preparation condition constant in embodiment 1, in step B the reactor rotating speed is adjusted into 5000rpm, the feed rate of peristaltic pump is increased to 620ml/min.The BaSO that finally obtains 4Median size is 32nm.
Embodiment 7:
Keep other preparation condition constant in embodiment 1, the gap with full back-mixing liquid film reactor in step B is adjusted into 0.1mm, and the reactor rotating speed is adjusted into 3000rpm, and the feed rate of peristaltic pump is adjusted into 150ml/min.The BaSO that finally obtains 4Median size is 65nm.
Embodiment 8:
Keep other preparation condition constant in embodiment 7, the maintenance rotating speed is 3000rpm, and the adjustment reactor gap is 0.2mm, and the feed rate of peristaltic pump is increased to 180ml/min.The BaSO that finally obtains 4Median size is 53nm.
Embodiment 9:
Keep other preparation condition constant in embodiment 7, the maintenance rotating speed is 3000rpm, and the adjustment reactor gap is 0.4mm, and the feed rate of peristaltic pump is increased to 370ml/min.The BaSO that finally obtains 4Median size is 38nm.
Embodiment 10:
Keep other preparation condition constant in embodiment 7, the maintenance rotating speed is 3000rpm, and the adjustment reactor gap is 0.5mm, and the feed rate of peristaltic pump is increased to 510ml/min.The BaSO that finally obtains 4Characterize through TEM, see Fig. 2 d, recording median size is 30nm.

Claims (3)

1. the method for preparing nano barium sulfate of a controllable particle size distribution, concrete preparation method is as follows:
A. the soluble barium salt is dissolved in that compound concentration is the barium salt solution of 0.01-1.3M in the deionized water; Soluble sulphate or sulfuric acid are dissolved in the deionized water, and compound concentration is vitriol or the sulphuric acid soln of 0.01-1.3M;
B. the gap width of adjusting between full back-mixing liquid film reactor rotor and the stator is 0.1-0.5mm, rotating speed is 1000-5000rpm, after the question response device stabilization of speed, with the feed rate of 150-620ml/min mol ratio barium salt solution and vitriol or sulphuric acid soln are added in the full back-mixing liquid film reactor, be carried out to nuclear reaction by 1:1; Be connected with 25 ℃ water of condensation in the reaction process in the maintenance outer stator chuck;
C. collect suspension slurry from reactor outlet, filter, exist with deionized water centrifuge washing to aqueous phase inclusion-free ion; The gained filter cake was placed the 60-80 ℃ of dry 10-15 of baking oven hour, and obtaining median size is 30-120nm nanometer BaSO 4
2. the method for preparing nano barium sulfate of a controllable particle size distribution is characterized in that the used soluble barium salt of steps A is BaCl 22H 2O, BaS, Ba (NO 3) 2Or BaCl 2, its purity is analytical pure; Used soluble sulphate is Na 2SO 4, MgSO 4, ZnSO 4Or AlSO 4, its purity is analytical pure; Used sulfuric acid is 98% the vitriol oil; The electric conductivity of used deionized water is not more than 10 -6S/cm.
3. the method for preparing nano barium sulfate of a controllable particle size distribution is characterized in that step B rotor rotating speed is gap between 4000-5000rpm, rotor and the stator when being 0.4-0.5mm, the BaSO of preparation 4Median size is 30-40nm.
CNA2008102267384A 2008-11-21 2008-11-21 Method for preparing nano barium sulfate with controllable particle size distribution Pending CN101423239A (en)

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CN102167386A (en) * 2011-03-16 2011-08-31 清华大学 Method for preparing barium sulfate nanoparticles
CN102351233A (en) * 2011-07-22 2012-02-15 中南大学 Production process for nanometer barium sulfate
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CN104195589A (en) * 2014-08-21 2014-12-10 成都新柯力化工科技有限公司 Preparation method and application of nano barium sulphate
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CN103864128A (en) * 2014-01-23 2014-06-18 永新股份（黄山）包装有限公司 Micron-grade barium sulfate particle and synthesis method thereof
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CN104195589A (en) * 2014-08-21 2014-12-10 成都新柯力化工科技有限公司 Preparation method and application of nano barium sulphate
CN104195589B (en) * 2014-08-21 2016-05-11 成都新柯力化工科技有限公司 A kind of preparation method of nano barium sulfate and application
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CN109052449A (en) * 2018-10-23 2018-12-21 贵州微化科技有限公司 A method of continuously preparing hydrogen sulfide coproduction nano barium sulfate using microreactor
CN110330046A (en) * 2019-05-21 2019-10-15 河北辛集化工集团有限责任公司 The technique that nano barium sulfate is prepared by microreactor as raw material using barium carbonate
CN110294487A (en) * 2019-05-29 2019-10-01 清华大学 A kind of microreactor prepares the new process of polymolecularity barium sulfate material
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