CN108479737A - A kind of preparation process of inorganic mineral material meso-hole structure - Google Patents

A kind of preparation process of inorganic mineral material meso-hole structure Download PDF

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Publication number
CN108479737A
CN108479737A CN201810233467.9A CN201810233467A CN108479737A CN 108479737 A CN108479737 A CN 108479737A CN 201810233467 A CN201810233467 A CN 201810233467A CN 108479737 A CN108479737 A CN 108479737A
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hole structure
slurry
inorganic mineral
mineral material
preparation process
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侯晓旭
徐前进
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Jiangxi Dehong Environmental Protection Technology Co Ltd
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Jiangxi Dehong Environmental Protection Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The present invention relates to technical field of mesoporous materials, more particularly to a kind of preparation process of inorganic mineral material meso-hole structure, include mainly Mechanical Crushing, second-time breakage, mixed pulp, magnetic separation, be dispersed with stirring, mixed acid solution, modified stirring, pressure filtration washing drying and final mechanical comminution process is added, finally obtains inorganic mineral material meso-hole structure.The meso-hole structure material surface activity produced by the production method is higher, and aperture is effectively controlled in macropore range, has very high use value.A kind of raw material of present invention offer are simple, and technological parameter is easy to control, and technological process is simple, at low cost, are suitable for industry or large-scale production.

Description

A kind of preparation process of inorganic mineral material meso-hole structure
Technical field
The present invention relates to technical field of mesoporous materials, more particularly to a kind of preparation work of inorganic mineral material meso-hole structure Skill.
Background technology
Inorganic porous material has bigger specific surface area and Kong Rong, in fine chemistry industry, petroleum and natural gas processing, inhales It is attached with detach equal fields and there is extensive purposes, wherein mesoporous material to have preferable foreground in the industrial production, according to mesoporous material The order of material can be divided into ordered mesoporous material and unordered mesoporous material to classify.
Ordered mesoporous material is the self-assembled structures that are formed using surfactant as template, by organic-inorganic circle Orientation between face, the porous material that assembly hole is structurally ordered and aperture is between 2-50nm, pore-size distribution is narrow, at present relatively Ripe material is M41S series silicon-based mesoporous molecular sieves, but pure silica does not have chemism, needs in application process Change the chemical composition of material.The aperture shape of unordered mesoporous material is complicated, it is irregular, be connected to each other, representative products have dioxy SiClx aeroge, devitrified glass etc..However, the synthesis technology of these materials is complicated, the control requirement to temperature, pressure and other parameters Very strict, cost is higher.The comprehensive current situation for summarizing current mesoporous material is exactly to face existing mesoporous material chemistry to live The low and high production cost problem of property, this is also a problem to be solved.
Based on the above current situation, it is necessary to which a kind of raw material are simple, at low cost, and technological process is simple, are suitable for big rule The preparation process with the active meso-hole structure material of high surfaces of mould production, to meet the market demand.
Invention content
In view of problem above, the present invention provides a kind of preparation works with the active meso-hole structure material of high surfaces Skill, raw material needed for the technique are simple, and at low cost, technological process is simple, are suitable for large-scale production, can expire to a certain extent The sufficient market demand.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
A kind of preparation process of inorganic mineral material meso-hole structure, includes the following steps in the present invention：
S1：Natural crystal preliminary mechanical is broken into the smaller stone of grain size, then carries out second-time breakage, be made grain size 1~ 100 microns of powdered granule；
S2：Add water to be mixed into the slurry that solid content is 20~50wt% the ore powdered granule that step S1 is obtained, carries out Grinding；
S3：In the slurry obtained into step S2 plus water is configured to the slurry that solid content is 10~40wt%, then vertical Magnetic separation is carried out on ring magnetic separator, is repeated 2~3 times；
S4：A certain amount of dispersant is added in the slurry obtained to step S3, is dispersed with stirring, wherein the amount of dispersant is slurry 1~3wt% of solid content in material；
S5：Hydrochloric acid and sulfuric acid mixed acid solution are added in the slurry of step S4, and improves temperature to 50~80 DEG C, stirs 1 ~4h；Wherein the addition of mixed acid solution is 10~40wt% of solid content in slurry；
S6：It is 7~8 that the slurry of step S5, which is adjusted pH, is stirred after modifying agent is added, 2000~4000rpm of rotating speed, Stir 20~40min；Wherein, the amount that modifying agent is added is 2~6wt% of solid content in slurry；
S7：By the slurry of step S6 by filter press press filtration, washing, obtained after separation of solid and liquid solid content be 20~ The filter cake of 40wt%；
S8：By filtration cakes torrefaction, siccative is obtained；
S9：The siccative that step S8 is obtained carries out mechanical crushing, obtains inorganic mineral material meso-hole structure.
Preferably, it is ground using sand milling dispersion machine in the step S2, frosting dispersion machine is used in the step S6 It is stirred.
Preferably, the rotating speed that dispersion machine is sanded in the step S2 is 700~1000rpm, and mixing time is 1~2h.
Preferably, the step S3 neutrality ring magnetic separators set magnetic field intensity as 10000~20000Gs.
Preferably, it after dispersant being added in the step S4, is dispersed with stirring using ball-milling dispersion machine, the ball-milling dispersion machine Rotating speed be 2000~5000rpm, 20~40min of mixing time.
Preferably, dispersant used in the step S4 is polycarboxylate sodium, calgon, sodium pyrophosphate, poly- third Olefin(e) acid sodium salt, one or more of polyvinyl alcohol.
Preferably, the mass ratio of the mixed acid solution composition used in the step S5 is hydrochloric acid:Sulfuric acid=0~10:20~ 40。
Preferably, modifying agent used in the step S6 is sodium sulfate of polyethenoxy ether of fatty alcohol (AES), coconut oleoyl amine Propyl betaine (CAB), gamma-aminopropyl-triethoxy-silane (KH550), γ-mercaptopropyl trimethoxysilane (KH580), ten One or more of sodium dialkyl sulfate (K12), dodecyl sodium sulfate.
Preferably, the drying temperature of filtration cakes torrefaction is 100~150 DEG C in the step S8, and drying time is 4~6h.
Preferably, the time for carrying out mechanical crushing in the step S9 to siccative is 1~5min.
The advantages of the present invention are：There is provided that a kind of raw material are simple, and technological parameter is easy to control, technique stream Journey is simple, at low cost, is suitable for industry or large-scale production.It is lived by the meso-hole structure material surface that the production method is produced Property it is higher, aperture is effectively controlled in macropore range, have very high use value.
Specific implementation mode
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more Add and clearly demonstrate technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
S1：Natural crystal preliminary mechanical is broken into the smaller stone of grain size, then carries out second-time breakage, and grain size 1~100 is made The powdered granule of micron；
S2：Water is added to be mixed into the slurry that solid content is 20wt% the ore powdered granule that step S1 is obtained, using sand milling Dispersion machine is ground；The rotating speed that dispersion machine is wherein sanded is 800rpm, mixing time 2h；
S3：In the slurry obtained into step S2 plus water is configured to the slurry that solid content is 10wt%, then in vertical ring type Magnetic separation is carried out on magnetic separator, is repeated 3 times；Wherein magnetic field intensity is 20000Gs；
S4：Dispersant is added in the slurry obtained to step S3, and is dispersed with stirring using ball-milling dispersion machine；Wherein dispersant Amount be solid content in slurry 2wt%, dispersant used is polycarboxylate sodium, and the rotating speed of ball-milling dispersion machine is 5000rpm, Mixing time 40min；
S5：Mixed acid solution is added in the slurry of step S4, and improves temperature to 80 DEG C, stirs 2h；Wherein mixed acid solution Addition be slurry in solid content 30wt%, nitration mixture composition mass ratio be hydrochloric acid:Sulfuric acid=10:40；
S6：It is 7 that the slurry of step S5, which is adjusted pH, and modifying agent is added, then frosting dispersion machine is used to stir, rotating speed 2000 ~4000rpm stirs 20~40min；Wherein, the amount that modifying agent is added is 2~6wt% of solid content in slurry, and used changes Property agent be gamma-aminopropyl-triethoxy-silane (KH550)；
S7：By the slurry of step S6 by filter press press filtration, washing, it is 30wt%'s that solid content is obtained after separation of solid and liquid Filter cake；
S8：By filtration cakes torrefaction, siccative is obtained；Wherein drying temperature is 150 DEG C, drying time 4h；
S9：The siccative that step S8 is obtained carries out mechanical crushing, obtains inorganic mineral material meso-hole structure；When wherein crushing Between be 2min.Finally, the meso-hole structure material obtained, specific surface area 70.86m2/ g, hole hold 0.28ml/g, aperture 13.71nm。
Embodiment 2
S1：Natural crystal preliminary mechanical is broken into the smaller stone of grain size, then carries out second-time breakage, and grain size 1~100 is made The powdered granule of micron；
S2：Water is added to be mixed into the slurry that solid content is 25wt% the ore powdered granule that step S1 is obtained, using sand milling Dispersion machine is ground；The rotating speed that dispersion machine is wherein sanded is 1000rpm, mixing time 2h；
S3：In the slurry obtained into step S2 plus water is configured to the slurry that solid content is 10wt%, then in vertical ring type Magnetic separation is carried out on magnetic separator, is repeated 3 times；Wherein magnetic field intensity is 20000Gs；
S4：Dispersant is added in the slurry obtained to step S3, and is dispersed with stirring using ball-milling dispersion machine；Wherein dispersant Amount be solid content in slurry 1wt%, dispersant used is polyvinyl alcohol, and the rotating speed of ball-milling dispersion machine is 5000rpm, is stirred Mix time 40min；
S5：Mixed acid solution is added in the slurry of step S4, and improves temperature to 80 DEG C, stirs 4h；Wherein mixed acid solution Addition be slurry in solid content 10wt%, nitration mixture composition mass ratio be hydrochloric acid:Sulfuric acid=0:1；
S6：It is 8 that the slurry of step S5, which is adjusted pH, and modifying agent is added, then frosting dispersion machine is used to stir, rotating speed 4000rpm stirs 40min；Wherein, the amount that modifying agent is added is the 4wt% of solid content in slurry, and modifying agent used is 12 Sodium alkyl sulfate (K12)；
S7：By the slurry of step S6 by filter press press filtration, washing, it is 28wt%'s that solid content is obtained after separation of solid and liquid Filter cake；
S8：By filtration cakes torrefaction, siccative is obtained；Wherein drying temperature is 105 DEG C, drying time 6h；
S9：The siccative that step S8 is obtained carries out mechanical crushing, obtains inorganic mineral material meso-hole structure；When wherein crushing Between be 5min.Finally, the meso-hole structure material obtained, specific surface area 89.27m2/ g, hole hold 0.69ml/g, aperture 26.85nm。
Embodiment 3
S1：Natural crystal preliminary mechanical is broken into the smaller stone of grain size, then carries out second-time breakage, and grain size 1~100 is made The powdered granule of micron；
S2：Water is added to be mixed into the slurry that solid content is 30wt% the ore powdered granule that step S1 is obtained, using sand milling Dispersion machine is ground；The rotating speed that dispersion machine is wherein sanded is 700rpm, mixing time 1h；
S3：In the slurry obtained into step S2 plus water is configured to the slurry that solid content is 20wt%, then in vertical ring type Magnetic separation is carried out on magnetic separator, is repeated 2 times；Wherein magnetic field intensity is 10000Gs；
S4：Dispersant is added in the slurry obtained to step S3, and is dispersed with stirring using ball-milling dispersion machine；Wherein dispersant Amount be solid content in slurry 1~3wt%, dispersant used is calgon, and the rotating speed of ball-milling dispersion machine is 2000rpm, mixing time 20min；
S5：Mixed acid solution is added in the slurry of step S4, and improves temperature to 50 DEG C, stirs 1h；Wherein mixed acid solution Addition be slurry in solid content 10wt%, nitration mixture composition mass ratio be hydrochloric acid:Sulfuric acid=1:2；
S6：It is 7 that the slurry of step S5, which is adjusted pH, and modifying agent is added, then frosting dispersion machine is used to stir, rotating speed 2000rpm stirs 20min；Wherein, the amount that modifying agent is added is the 2wt% of solid content in slurry, and modifying agent used is cocounut oil Amido propyl betaine (CAB)；
S7：By the slurry of step S6 by filter press press filtration, washing, it is 40wt%'s that solid content is obtained after separation of solid and liquid Filter cake；
S8：By filtration cakes torrefaction, siccative is obtained；Wherein drying temperature is 150 DEG C, drying time 4h；
S9：The siccative that step S8 is obtained carries out mechanical crushing, obtains inorganic mineral material meso-hole structure；When wherein crushing Between be 1min.Finally, the meso-hole structure material obtained, specific surface area 54.28m2/ g, hole hold 0.26ml/g, aperture 16.94nm。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.

Claims (10)

1. a kind of preparation process of inorganic mineral material meso-hole structure, which is characterized in that mainly include the following steps that：
S1：Natural crystal preliminary mechanical is broken into the smaller stone of grain size, then carries out second-time breakage, it is micro- that grain size 1~100 is made The powdered granule of rice；
S2：Add water to be mixed into the slurry that solid content is 20~50wt% the ore powdered granule that step S1 is obtained, is ground；
S3：In the slurry obtained into step S2 plus water is configured to the slurry that solid content is 10~40wt%, then in vertical ring type Magnetic separation is carried out on magnetic separator, is repeated 2~3 times；
S4：A certain amount of dispersant is added in the slurry obtained to step S3, is dispersed with stirring, wherein the amount of dispersant is in slurry 1~3wt% of solid content；
S5：Hydrochloric acid and sulfuric acid mixed acid solution are added in the slurry of step S4, and improves temperature to 50~80 DEG C, stirs 1~4h； Wherein, the addition of mixed acid solution is 10~40wt% of solid content in slurry；
S6：It is 7~8 that the slurry of step S5, which is adjusted pH, is stirred after modifying agent is added, 2000~4000rpm of rotating speed, stirring 20~40min；Wherein, the amount that modifying agent is added is 2~6wt% of solid content in slurry；
S7：By the slurry of step S6 by filter press press filtration, washing, it is 20~40wt%'s that solid content is obtained after separation of solid and liquid Filter cake；
S8：By filtration cakes torrefaction, siccative is obtained；
S9：The siccative that step S8 is obtained carries out mechanical crushing, finally obtains inorganic mineral material meso-hole structure.
2. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step It is ground using sand milling dispersion machine in rapid S2, is stirred using frosting dispersion machine in the step S6.
3. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step The rotating speed that dispersion machine is sanded in rapid S2 is 700~1000rpm, and mixing time is 1~2h.
4. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step Rapid S3 neutrality ring magnetic separators set magnetic field intensity as 10000~20000Gs.
5. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step After dispersant is added in rapid S4, it is dispersed with stirring using ball-milling dispersion machine, the rotating speed of the ball-milling dispersion machine is 2000~ 5000rpm, 20~40min of mixing time.
6. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step Dispersant used in rapid S4 is in polycarboxylate sodium, calgon, sodium pyrophosphate, polyacrylic acid sodium salt and polyvinyl alcohol It is one or more of.
7. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step The mass ratio of the mixed acid solution composition used in rapid S5 is hydrochloric acid:Sulfuric acid=0~10:20~40.
8. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step Modifying agent used in rapid S6 is sodium sulfate of polyethenoxy ether of fatty alcohol, Cocoamidopropyl betaine, three ethoxy of γ-aminopropyl One or more of base silane, γ-mercaptopropyl trimethoxysilane, lauryl sodium sulfate, dodecyl sodium sulfate.
9. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that the step The drying temperature of filtration cakes torrefaction is 100~150 DEG C in rapid S8, and drying time is 4~6h.
10. a kind of preparation process of inorganic mineral material meso-hole structure according to claim 1, which is characterized in that described The time for carrying out mechanical crushing in step S9 to siccative is 1~5min.
CN201810233467.9A 2018-03-21 2018-03-21 A kind of preparation process of inorganic mineral material meso-hole structure Pending CN108479737A (en)

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Publication number Priority date Publication date Assignee Title
CN101007635A (en) * 2007-01-19 2007-08-01 华南理工大学 Organic-pillared vermiculite mesoporous material and its preparing process and uses
CN100591741C (en) * 2004-07-20 2010-02-24 埃尔凯姆有限公司 Granules of powdery mineral and method for production of granules

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100591741C (en) * 2004-07-20 2010-02-24 埃尔凯姆有限公司 Granules of powdery mineral and method for production of granules
CN101007635A (en) * 2007-01-19 2007-08-01 华南理工大学 Organic-pillared vermiculite mesoporous material and its preparing process and uses

Non-Patent Citations (2)

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Title
刘东等: "《重庆晚二叠世煤系地层稀有金属矿床开发利用研究——以中梁山为例》", 30 November 2017, 中国地质大学出版社 *
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Application publication date: 20180904