CN110368918A - A kind of Spray granulation method of boehmite powder - Google Patents

A kind of Spray granulation method of boehmite powder Download PDF

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Publication number
CN110368918A
CN110368918A CN201910752465.5A CN201910752465A CN110368918A CN 110368918 A CN110368918 A CN 110368918A CN 201910752465 A CN201910752465 A CN 201910752465A CN 110368918 A CN110368918 A CN 110368918A
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powder
boehmite powder
spray granulation
boehmite
granulation method
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Inventor
宋元江
李文龙
李扬
董玲玉
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Southwest Research and Desigin Institute of Chemical Industry
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Southwest Research and Desigin Institute of Chemical Industry
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02Boron or aluminium; Oxides or hydroxides thereof
    • B01J21/04Alumina
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0018Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027Powdering
    • B01J37/0045Drying a slurry, e.g. spray drying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0063Granulating

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The present invention provides a kind of Spray granulation method of boehmite powder, belongs to shaping of catalyst technical field.It include: 1) ingredient: in terms of slurries gross mass, boehmite powder, sintering aid, binder, dispersing agent are weighed according to following mass fraction: 35~50wt% of boehmite powder, 2.5~5.5wt% of sintering aid, 1.0~4.0wt% of binder, 1.0~4.0wt% of dispersing agent, deionized water is added, heating water bath and stirring are made into the stable dispersion slurries that solid content is 38~55%;2) mist projection granulating: obtained slurries are directly sprayed in people's pelletizer, and control atomizing granulating technology parameter obtains being granulated powder.The mist projection granulating powder particles being prepared using the method for the present invention are in regular ball, and porous media is uniform, centralized particle diameter and controllable.Mist projection granulating powder mobility, compactness and reproducible can carry out continuous automatic moulding it is not necessary that lubricant is added, and save the cost improves production efficiency.

Description

A kind of Spray granulation method of boehmite powder
Technical field
The invention belongs to shaping of catalyst technical field, specially a kind of Spray granulation method of boehmite powder.
Background technique
Boehmite also known as false boehmite, nontoxic, tasteless, odorless, white powder, with specific surface area Greatly, with high purity, anticorrosive good, it is a kind of important large Inorganic Chemicals, in chemical industry catalysis, petroleum hydrofinishing, synthesis The catalyst fields such as chlorine, car tail gas purification are widely used, and are mainly used as production catalyst carrier --- the original of activated alumina Material.
With the development of boehmite moulding process, people to how to prepare high-performance boehmite and its it is related at Type technical study is more and more, specifically how prepares that a kind of good fluidity, particle is spherical in shape, particle diameter distribution is uniform, compactness Good powder body material is more by the favor of researcher.Spray granulation is mentioned with to powder body material building-up property requirement Height starts to be applied to catalyst carrier forming field.Carrying out mist projection granulating to boehmite slurry not only can be to avoid each component Reunite again and sedimentation separation, maintain the original uniformity of slurry;Slurry atomization is uniform simultaneously, obtains regular shape, partial size It is evenly distributed, good fluidity and the granulation powder for being suitble to continuous automatic moulding.The production efficiency for improving catalyst carrier, more has Conducive to the uniformity, stability and anti-sintering property of carrier quality, the service life of catalyst is extended, is brought more to enterprise More economic benefits has good prospects for commercial application.
Summary of the invention
The purpose of the present invention is to provide a kind of Spray granulation methods of boehmite powder.Boehmite after spraying Powder fluidity greatly improves, and diameter of particle is evenly distributed, compactness is good, is appropriate for continuous automatic moulding, produces high quality Catalyst carrier.
The object of the invention is achieved through the following technical solutions:
A kind of Spray granulation method of boehmite powder, comprising the following steps:
1) ingredient: in terms of slurries gross mass, by boehmite powder, sintering aid, binder, dispersing agent according to following matter Amount score is weighed: boehmite 35~50wt% of powder, 2.5~5.5wt% of sintering aid, and binder 1.0~ Deionized water is added in 4.0wt%, 1.0~4.0wt% of dispersing agent, and it is 38~55% that heating water bath and stirring, which are made into solid content, Stable dispersion slurries;
2) mist projection granulating: obtained slurries are directly sprayed in people's pelletizer, and control atomizing granulating technology parameter is granulated Powder.
Further, the sintering aid is one of clay, bentonite, kaolin or a variety of.It is preferred that sintering aid energy The mechanical strength for enough improving powder tabletting carrier, reduces the rate of wear of catalyst, extends the service life of catalyst.
Further, the binder is polyvinyl alcohol (PVA), silica solution, ammonium polyacrylate, hydroxypropyl methyl cellulose (HPMC), one of aluminum magnesium silicate or a variety of.Preferred binder can enhance the viscosity of slurries phase, form netted knot in water Structure effectively delays the generation of powder sedimentation, coalescence, improves the stability of slurries.
Further, the dispersing agent is polyethylene glycol (PEG), sodium carboxymethylcellulose (CMC-Na), methylcellulose (MC), one of polyvinylpyrrolidone (PVP), naphthalene sulfonate D-425 or a variety of.Preferred dispersants can be adsorbed on powder Particle surface acts on forming stronger protective barrier by steric hindrance, prevents powder particles from assembling again, and make powder particles Surface is easy to soak, and keeps the dispersion of each substance in slurries more uniform, stable.
Further, in terms of slurries gross mass, the mass fraction of the sintering aid each component is clay: 0.0~ 3.5wt%, bentonite: 0.0~3.0wt%, kaolin: 0.0~4.0wt%.
Further, in terms of slurries gross mass, the mass fraction of the binder each component is polyvinyl alcohol (PVA): 0.0~ 1.5wt%, silica solution: 0.0~1.5wt%, ammonium polyacrylate: 0.0~0.6wt%, hydroxypropyl methyl cellulose (HPMC): 0.0~1.8wt%, aluminum magnesium silicate: 0.0~0.8wt%.
Further, in terms of slurries gross mass, the mass fraction of the dispersing agent each component is polyethylene glycol (PEG): 0.0~ 1.5wt%, sodium carboxymethylcellulose (CMC-Na): 0.0~1.0wt%, methylcellulose (MC): 0.0~2.0wt%, poly- second Alkene pyrrolidone (PVP): 0.0~1.5wt%, naphthalene sulfonate D-425:0.0~1.0wt.
Further, the water bath heating temperature is 70~95 DEG C, and mixing time is 1~3h.Water-bath can improve in solution The effect of the surface hydroxyl of hydrogen ion and boehmite, improves the sour dispersion index of boehmite.
Further, the sponging granulator is air-flowing type sponging granulator, and inlet temperature is 240~270 DEG C, outlet temperature It is 120~150 DEG C, feed rate 55rap/min, dry intraventricular pressure difference is 30~55Pa.Preferably air-stream spraying pelletizer The contact of gas-liquid two-phase is more flexible when making spraying, it is ensured that droplet has enough residence times;Spray drying tower is smaller, structure Simply, easy to process;Atomizer operating is convenient, can easily be accommodated.
A kind of boehmite powder, is prepared using method described above.
Compared with prior art, the invention has the following advantages:
It is in regular ball using the mist projection granulating powder particles that the method for the present invention is prepared, porous media is uniform, grain Diameter distribution is concentrated and controllable.
The mist projection granulating powder mobility that is prepared using the method for the present invention, compactness and reproducible, without being added Lubricant can carry out continuous automatic moulding, and save the cost improves production efficiency.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Embodiment 1
1, weigh 450.0g boehmite powder, 36.0g clay, 9.0g PVA, 4.5g aluminum magnesium silicate, 9.0g PEG, 563.0g deionized water is added in 6.75g PVP, 4.5g naphthalene sulfonate D-425, and heating water bath is to 75 DEG C and stirs 2h, is made into solid The stable dispersion slurries that content is 48%.
In terms of slurries gross mass, wherein boehmite powder accounts for 41.56%, and clay accounts for 3.32%, PVA and accounts for 0.83%, silicon Sour magnalium, which accounts for 0.42%, PEG and accounts for 0.83%, PVP, accounts for 0.62%, and naphthalene sulfonate D-425 accounts for 0.42%;
2, above-mentioned slurries are injected directly into air-flowing type sponging granulator, inlet temperature is 260 DEG C, outlet temperature 150 DEG C, feed rate 55rap/min, dry intraventricular pressure difference is 30~55Pa, obtains mist projection granulating powder, number 1#.
Embodiment 2
1, weigh 450.0g boehmite powder, 13.5g clay, 31.5g kaolin, 13.5g PVA, 4.5g HPMC, 9.0g PEG, 9.0g CMC-Na, 4.5g PVP are weighed in proportion, be added 580.13g deionized water, heating water bath to 85 DEG C simultaneously 2.5h is stirred, the stable dispersion slurries that solid content is 48% are made into.
In terms of slurries gross mass, wherein boehmite powder accounts for 40.34%, and clay accounts for 1.21%, and kaolin accounts for 2.82%, PVA, which accounts for 1.21%, HPMC and accounts for 0.40%, PEG and account for 0.81%, CMC-Na and account for 0.81%, PVP, accounts for 0.40%;
2, above-mentioned slurries are injected directly into air-flowing type sponging granulator, inlet temperature is 250 DEG C, outlet temperature 140 DEG C, feed rate 55rap/min, dry intraventricular pressure difference is 30~55Pa, obtains mist projection granulating powder, number 2#.
Embodiment 3
1,450.0g boehmite powder, 31.5g bentonite, 22.5g kaolin, 13.5g silica solution, 9.0g are weighed HPMC, 6.75g aluminum magnesium silicate, 18.0g MC, 13.5g PVP, 9.0g naphthalene sulfonate D-425 are weighed in proportion, and 673.53g is added Deionized water, heating water bath is to 90 DEG C and stirs 2.5h, is made into the stable dispersion slurries that solid content is 46%.
In terms of slurries gross mass, wherein boehmite powder accounts for 36.08%, and bentonite accounts for 2.53%, and kaolin accounts for 1.80%, silica solution accounts for 1.08%, HPMC and accounts for 0.72%, and aluminum magnesium silicate, which accounts for 0.54%, MC and accounts for 1.44%, PVP, accounts for 1.08%, naphthalene Sulfonate D-425 accounts for 0.72%;
2, above-mentioned slurries are injected directly into air-flowing type sponging granulator, inlet temperature is 270 DEG C, outlet temperature 130 DEG C, feed rate 55rap/min, dry intraventricular pressure difference is 30~55Pa, obtains mist projection granulating powder, number 3#.
Embodiment 4
1,450.0g boehmite powder, 27.0g clay, 18.0g bentonite, 13.5g PVA, 4.5g polyacrylic acid are weighed Ammonium, 9.0g HPMC, 4.5g aluminum magnesium silicate, 13.5g PEG, 4.5g MC, 4.5g PVP are weighed in proportion, be added 549.0g go from Sub- water, heating water bath is to 80 DEG C and stirs 3h, is made into the stable dispersion slurries that solid content is 50%.
In terms of slurries gross mass, wherein boehmite powder accounts for 40.98%, and clay accounts for 2.46%, and bentonite accounts for 1.64%, PVA accounts for 1.23%, and ammonium polyacrylate accounts for 0.41%, HPMC and accounts for 0.82%, and aluminum magnesium silicate, which accounts for 0.41%, PEG and accounts for 1.23%, MC, to be accounted for 0.41%, PVP account for 0.41%;
2, above-mentioned slurries are injected directly into air-flowing type sponging granulator, inlet temperature is 240 DEG C, outlet temperature 120 DEG C, feed rate 55rap/min, dry intraventricular pressure difference is 30~55Pa, obtains mist projection granulating powder, number 4#.
Embodiment 5
1, weigh 450.0g boehmite powder, 13.5g clay, 36.0g kaolin, 9.0g PVA, 13.5g silica solution, 13.5g HPMC, 4.5g PEG, 9.0g MC, 13.5g PVP, 9.0g naphthalene sulfonate D-425 are weighed in proportion, and 644.46g is added Deionized water, heating water bath is to 80 DEG C and stirs 3h, is made into the stable dispersion slurries that solid content is 47%.
In terms of slurries gross mass, wherein boehmite powder accounts for 37.01%, and clay accounts for 1.11%, and kaolin accounts for 2.96%, PVA accounts for 0.74%, and silica solution, which accounts for 1.11%, HPMC and accounts for 1.11%, PEG and account for 0.37%, MC and account for 0.74%, PVP, accounts for 1.11%, naphthalene Sulfonate D-425 accounts for 0.74%;
2, above-mentioned slurries are injected directly into air-flowing type sponging granulator, inlet temperature is 250 DEG C, outlet temperature 130 DEG C, feed rate 55rap/min, dry intraventricular pressure difference is 30~55Pa, obtains mist projection granulating powder, number 5#.
Embodiment 6
1, weigh 450.0g boehmite powder, 13.5g clay, 36.0g kaolin, 9.0g PVA, 13.5g silica solution, 13.5g HPMC, 4.5g PEG, 9.0g MC, 13.5g PVP, 9.0g naphthalene sulfonate D-425 are weighed in proportion, and 644.46g is added Deionized water, heating water bath is to 30 DEG C and stirs 1h, is made into the stable dispersion slurries that solid content is 47%.
In terms of slurries gross mass, wherein boehmite powder accounts for 37.01%, and clay accounts for 1.11%, and kaolin accounts for 2.96%, PVA accounts for 0.74%, and silica solution, which accounts for 1.11%, HPMC and accounts for 1.11%, PEG and account for 0.37%, MC and account for 0.74%, PVP, accounts for 1.11%, naphthalene Sulfonate D-425 accounts for 0.74%;
2, above-mentioned slurries are injected directly into air-flowing type sponging granulator, inlet temperature is 210 DEG C, outlet temperature 100 DEG C, feed rate 40rap/min, dry intraventricular pressure difference is 65Pa, obtains mist projection granulating powder, number 6#.
Mist projection granulating powder and the test of original powder partial size
Partial size test method: taking 4g powder to be put into 20ml graduated cylinder, and 15g deionized water is added, and is stirred with plastic dropper equal It is even and take 3ml solution sample, each sample powder particle size is tested using laser particle size analyzer.
Test result is as follows shown in table 1 for 1 to 6 mist projection granulating powder of embodiment and the partial size of original powder.
1 embodiment of table, 1 to 6 mist projection granulating powder and original powder partial size test result
Number 1# 2# 3# 4# 5# 6# Original powder #
Partial size/μm 127.496 138.438 187.287 153.504 146.359 73.479 10.086
As shown in Table 1,1#~5# boehmite powder through mist projection granulating of the present invention processing after partial size much higher than spray 10.086 μm of original powder partial size before mist, powder mobility greatly improves, and automatic moulding performance is remarkably reinforced.6# boehmite powder Expect that atomizing granulating technology parameter does not limit in range in the present invention, though powder particle size is increased slightly compared with original powder partial size after spraying, It is obvious to be far below 2~3 times of powder particle size obtained through preferably atomizing granulating technology parameter of the invention.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (10)

1. a kind of Spray granulation method of boehmite powder, which comprises the following steps:
1) ingredient: in terms of slurries gross mass, by boehmite powder, sintering aid, binder, dispersing agent according to following quality point Number is weighed: boehmite 35~50wt% of powder, 2.5~5.5wt% of sintering aid, 1.0~4.0wt% of binder, point 1.0~4.0wt% of powder, is added deionized water, and heating water bath simultaneously stirs the stable dispersion slurry for being made into that solid content is 38~55% Liquid;
2) mist projection granulating: obtained slurries are directly sprayed in people's pelletizer, and control atomizing granulating technology parameter obtains being granulated powder.
2. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that the sintering aid For one of clay, bentonite, kaolin or a variety of.
3. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that the binder is One of polyvinyl alcohol (PVA), silica solution, ammonium polyacrylate, hydroxypropyl methyl cellulose (HPMC), aluminum magnesium silicate are more Kind.
4. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that the dispersing agent is Polyethylene glycol (PEG), sodium carboxymethylcellulose (CMC-Na), methylcellulose (MC), polyvinylpyrrolidone (PVP), naphthalene sulphur One of hydrochlorate D-425 or a variety of.
5. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that with slurries gross mass Meter, the mass fraction of the sintering aid each component are clay: 0.0~3.5wt%, bentonite: 0.0~3.0wt%, kaolinite Soil: 0.0~4.0wt%
6. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that with slurries gross mass Meter, the mass fraction of the binder each component are polyvinyl alcohol (PVA): 0.0~1.5wt%, silica solution: 0.0~ 1.5wt%, ammonium polyacrylate: 0.0~0.6wt%, hydroxypropyl methyl cellulose (HPMC): 0.0~1.8wt%, aluminum magnesium silicate: 0.0~0.8wt%.
7. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that with slurries gross mass Meter, the mass fraction of the dispersing agent each component are polyethylene glycol (PEG): 0.0~1.5wt%, sodium carboxymethylcellulose (CMC- Na): 0.0~1.0wt%, methylcellulose (MC): 0.0~2.0wt%, polyvinylpyrrolidone (PVP): 0.0~ 1.5wt%, naphthalene sulfonate D-425:0.0~1.0wt.
8. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that the heating water bath Temperature is 70~95 DEG C, and mixing time is 1~3h.
9. a kind of Spray granulation method of boehmite powder as described in claim 1, which is characterized in that the mist projection granulating Machine is air-flowing type sponging granulator, and inlet temperature is 240~270 DEG C, and outlet temperature is 120~150 DEG C, and feed rate is 55rap/min, dry intraventricular pressure difference are 30~55Pa.
10. a kind of boehmite powder, which is characterized in that using the described in any item method preparations of the claims 1 to 9 It obtains.
CN201910752465.5A 2019-08-15 2019-08-15 A kind of Spray granulation method of boehmite powder Pending CN110368918A (en)

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CN116265108A (en) * 2021-12-17 2023-06-20 中国石油天然气股份有限公司 Preparation method of catalytic cracking catalyst for producing more gasoline
CN116265107A (en) * 2021-12-17 2023-06-20 中国石油天然气股份有限公司 Preparation method of catalytic cracking catalyst for producing diesel oil in large quantity
CN116265106A (en) * 2021-12-17 2023-06-20 中国石油天然气股份有限公司 Preparation method of catalytic cracking catalyst for high yield of low carbon olefin

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ABHISEK CHOUDHARY等: ""Experimental Investigation on Flowability and Compaction Behavior of Spray Granulated Submicron Alumina Granules"", 《ISRN CERAMICS》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470522A (en) * 2020-03-31 2020-07-31 洛阳中超新材料股份有限公司 Spherical alumina and preparation method and application thereof
CN111470522B (en) * 2020-03-31 2021-12-07 洛阳中超新材料股份有限公司 Spherical alumina and preparation method and application thereof
CN116265108A (en) * 2021-12-17 2023-06-20 中国石油天然气股份有限公司 Preparation method of catalytic cracking catalyst for producing more gasoline
CN116265107A (en) * 2021-12-17 2023-06-20 中国石油天然气股份有限公司 Preparation method of catalytic cracking catalyst for producing diesel oil in large quantity
CN116265106A (en) * 2021-12-17 2023-06-20 中国石油天然气股份有限公司 Preparation method of catalytic cracking catalyst for high yield of low carbon olefin

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Application publication date: 20191025