CN107352565A - A kind of preparation method of boehmite - Google Patents

A kind of preparation method of boehmite Download PDF

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Publication number
CN107352565A
CN107352565A CN201710340688.1A CN201710340688A CN107352565A CN 107352565 A CN107352565 A CN 107352565A CN 201710340688 A CN201710340688 A CN 201710340688A CN 107352565 A CN107352565 A CN 107352565A
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China
Prior art keywords
acid
boehmite
solution
dead catalyst
washing
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Pending
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CN201710340688.1A
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Chinese (zh)
Inventor
郑淑琴
何理均
唐课文
张盼良
任邵
张建策
潘登
徐书伟
李洁
周永
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Hunan Institute of Science and Technology
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Hunan Institute of Science and Technology
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Priority to CN201710340688.1A priority Critical patent/CN107352565A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
    • B01J21/04—Alumina
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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

Abstract

The invention discloses a kind of preparation method of boehmite, a kind of method that boehmite is prepared using FCC dead catalyst, this preparation method is characterised by comprising the steps of：A）FCC dead catalyst is added in acid solution, after stirring and evenly mixing, 18 h is reacted at 50 90 DEG C, afterwards filtration washing, collects filtrate, obtain acid reaction liquid；B）The acid reaction liquid that step A is obtained, alkaline solution is added, fully after reaction, filtration washing, it is meta-aluminate solution to obtain filtrate；C）The obtained filtrates of step B are mixed with aluminum salt solution, regulation system pH=7.5 12, under stirring, 60 100 DEG C of h of aging 2 12, obtain reaction product；D）The reaction product that step C is obtained filters washing, is crushed after filtration cakes torrefaction, and boehmite is made.The present invention provides a kind of technical strategies to prepare the boehmite of high added value from FCC dead catalyst, can solve the problem of environmental pollution that FCC dead catalyst is brought.

Description

A kind of preparation method of boehmite
Technical field
It is a kind of using FCC dead catalyst to be former specifically the present invention relates to a kind of method for preparing boehmite Material, boehmite is made through processes such as peracid treatment, plastic, agings.Belong to field of inorganic material preparing technology.
Background technology
Boehmite also known as false boehmite, AlOOHnH 2O, n=0.08 ~ 0.62, its crystalline phase purity is high, peptization Performance is good, and caking property is strong, has the features such as higher than surface, pore volume is big.The binding agent of semi-synthetic catalytic cracking catalyst, silicon can be made The binding agent of sour aluminium refractory fibre, dehydration of alcohol catalyst for making ethylene and goes back oxidative ethane catalyst etc., can also make production catalyst The raw material of carrier, activated alumina and other aluminium salts, it is a kind of inorganic material with broad based growth future.
Boehmite industrially typically has three kinds of preparation methods：1）The neutralization reaction of aluminium salt and alkali, such as Alchlor process； 2）The metathesis reaction of aluminium salt and aluminate, such as aluminum sulfate method；3）The neutralization reaction of aluminate and acid, such as carbonizatin method.
A kind of method for preparing boehmite to discard Si-Al molecular sieve as raw material, this method have been invented in sea is refined et al. Comprise the following steps：First discarded Si-Al molecular sieve is well mixed with acid compound solution, reacted at 60-110 DEG C 0.5-10 h, filter to obtain acid reaction liquid and insoluble matter；Then obtained acid reaction liquid and alkaline precipitating agent are neutralized Plastic, after reaction terminates, above-mentioned slurries are handled into 2-6 h at 60-90 DEG C, separation of solid and liquid, washing, drying, obtain boehmite Powder.The invention replaces the expensive raw material of industry to prepare boehmite with discarded Si-Al molecular sieve, make discarded object as a means of Sourceization utilizes.The invention does not refer to the processing method of impurity element and the shadow to synthesizing boehmite in discarded Si-Al molecular sieve Ring.
A kind of method that boehmite is prepared by fast shedding be also invented in sea is refined et al., its step includes：1）In right amount A certain amount of dispersant is added in deionized water, then adds fast shedding, and it is crystal seed to add a small amount of boehmite, fully After stirring, control system pH values and thermotonus certain time；2）After reaction terminates, slurries are adjusted to alkalescence with ammoniacal liquor Burin-in process is carried out, then carries out separation of solid and liquid, is washed, is obtained the product cake of imurity-removal, finally dry product, obtain Boehmite powder.
Chen Yan is wide et al. to have invented a kind of method using coal ash for manufacturing for boehmite, and flyash is located in advance Reason；Flyash and Na after being pre-processed under high temperature2CO3Roasting obtains Silicon-rich gel and thick AlCl3Solution；Utilize thick AlCl3Solution system The sodium aluminate solution of standby purifying；The concentration for adjusting purifying sodium aluminate solution obtained above is 0.8-2.0 mol/L, is added Concentration is 0.8-2.0 mol/L NaHCO3Solution reaction plastic, product is under the conditions of 50-100 DEG C, pH values 7-11, always After changing 10-30 h, it is separated by filtration, obtains filter cake and filtered fluid；Using filter cake by the use of deionized water as washing lotion, wash, be dried to obtain Boehmite finished product.
A kind of method that boehmite is prepared using alunite has been invented by Lu Li armies et al., and its step includes：By alum Stone mixes the solution to form solid content 2-85 % with deionized water, and adding a kind of alkali makes aluminium separate out plastic, and control plastic is whole PH=7.5-12 of point, and the aging 0.5-100 h at 50-110 DEG C, washing, filter and dry.
The present invention passes through acid treatment, filtration washing, removal of impurities, plastic, aging, diafiltration excessively using FCC dead catalyst as raw material The process such as wash, dry, crushing and boehmite is made.
The content of the invention
It is an object of the invention to provide a kind of method that boehmite is prepared using FCC dead catalyst as raw material.We Method can enable discarded object recycling, improve its value, solve problem of environmental pollution.With very high economy effect Benefit and environmental benefit.
The invention discloses a kind of method for preparing boehmite, using FCC dead catalyst as raw material, it is characterised in that with Lower step：
A, FCC dead catalyst is added in acid solution, after stirring and evenly mixing, 1-8 h is reacted at 50-90 DEG C, are filtered afterwards Washing, filtrate is collected, obtains acid reaction liquid；
B, the acid reaction liquid for obtaining step A, alkaline solution is added, fully after reaction, filtration washing, it is meta-aluminic acid to obtain filtrate Salting liquid；
C, the filtrate that step B is obtained is mixed with aluminum salt solution, regulation system pH=7.5-12, under stirring, 60-100 DEG C aging 2-12 h, obtain reaction product；
D, the reaction product for obtaining step C filters washing, is crushed after filtration cakes torrefaction, that is, boehmite is made.
2nd, the method as described in claim 1, it is characterised in that in described step A, acid solution be hydrochloric acid, sulfuric acid, At least one of nitric acid, formic acid and acetic acid, the addition of acidic materials is itself and the reason that reactive aluminum is aoxidized in FCC dead catalyst By the 120-200 % of dosage, liquid-solid ratio is 3-10 L/kg.
3rd, the method as described in claim 1, it is characterised in that in described step B, alkaline solution is sodium hydroxide, hydrogen At least one of potassium oxide, ammoniacal liquor, the addition of alkaline matter is its theoretical amount with aluminium salt reaction in acid reaction liquid 150-200 %.
4th, the method as described in claim 1, it is characterised in that in described step C, aluminium salt Al2(SO4)3、Al2 (NO3)3、AlCl3In any one.
The inventive method has advantages below：1）Preparation process is simple, mild condition, easily implements industrialization；2） Boehmite prepared by the inventive method has crystallinity high, and alumina content is high, and uniform particle diameter is bigger than surface, and pore volume is big, The characteristics of pore distribution concentration, impurity content are few, show products application to before the development in the fields such as catalyst carrier, adsorbent Scape；3）The present invention prepares boehmite using FCC dead catalyst as raw material, substantially reduces the processing for preparing cost and solid waste Cost, while can solve pollution problem of the FCC dead catalyst to environment, meet China's changing rejected material to useful resource comprehensive utilization and environment Protect dual strategic requirement.
Embodiment
The present invention is described in further detail with reference to embodiment, but and is not so limited the present invention.
Embodiment 1
（1）500 g FCC dead catalyst are added into the g of hydrochloric acid solution 4652 that concentration is 6 mol/L, are warming up to 70 DEG C, reaction 3 h, filtered after the completion of reaction, obtain acid reaction liquid；
（2）By step（1）Obtained acid reaction liquid, addition concentration are the g of 31.6 % sodium hydroxide solutions 3872, fully reaction After the completion of, filtration washing, filtrate is sodium aluminate solution；
（3）By step（2）Obtained sodium aluminate solution mixes with the aluminum sulfate solution that alumina concentration is 90 g/L, adjusts body It is pH=9.5, under stirring, the h of aging 6 at 80 DEG C；
（4）By step（3）Obtained reaction product filtering washing, filter cake crush after drying 8 h at 120 DEG C, that is, it is thin that plan is made Diaspore A.
Embodiment 2
（1）100 g FCC dead catalyst are added into the g of concentrated hydrochloric acid solution 372, are warming up to 90 DEG C, 1 h are reacted, after the completion of reaction Filtering, obtains acid reaction liquid；
（2）By step（1）Obtained acid reaction liquid, addition concentration are the g of 17.1 % potassium hydroxide solutions 2284, fully reaction After the completion of, filtration washing, filtrate is potassium metaaluminate solution；
（3）By step（2）Obtained potassium metaaluminate solution mixes with the liquor alumini chloridi that alumina concentration is 25 g/L, adjusts body It is pH=12, under stirring, the h of aging 3 at 95 DEG C；
（4）By step（3）Obtained reaction product filtering washing, filter cake crush after drying 4 h at 150 DEG C, that is, it is thin that plan is made Diaspore B.
Embodiment 3
（1）1000 g FCC dead catalyst are added into the g of salpeter solution 8993 that concentration is 30 %, are warming up to 50 DEG C, processing 8 H, filtered after the completion of reaction, obtain acid reaction liquid；
（2）By step（1）Obtained acid reaction liquid, addition concentration are the g of 17.2 % ammonia spirits 16615, and fully reaction is completed Afterwards, filtration washing, filtrate are sodium aluminate solution；
（3）By step（2）Obtained sodium aluminate solution mixes with the aluminum nitrate solution that alumina concentration is 15 g/L, adjusts body It is pH=10, under stirring, the h of aging 12 at 60 DEG C；
（4）By step（3）Obtained reaction product filtering washing, filter cake crush after drying 6 h at 130 DEG C, that is, it is thin that plan is made Diaspore C.
Embodiment 4
（1）300g FCC dead catalyst is added into the g of acetum 1966 that concentration is 56 %, 80 DEG C is warming up to, handles 6 h, Filtered after the completion of reaction, obtain acid reaction liquid；
（2）By step（1）Obtained acid reaction liquid, addition concentration are the g of 31.6 % sodium hydroxides 2478, and fully reaction is completed Afterwards, filtration washing, filtrate are sodium aluminate solution；
（3）By step（2）Obtained sodium aluminate solution mixes with the aluminum sulfate solution that alumina concentration is 90 g/L, adjusts body It is pH=8.5, under stirring, the h of aging 2 at 100 DEG C；
（4）By step（3）Obtained reaction product filtering washing, filter cake crush after drying 10 h at 110 DEG C, that is, are made and intend Boehmite D.
The boehmite product property of table 1
Sample number into spectrum Than surface, m2/g Pore volume, ml/g Aperture, nm Aluminum oxide, m%
A 387 0.37 5.11 97.91
B 442 0.41 4.98 96.55
C 416 0.45 5.82 95.63
D 395 0.39 4.25 98.59
Commercial boehmite 357 0.37 3.78 91.58
It is high using the boehmite specific surface area prepared by the inventive method it can be seen from the property of table 1, pore volume and aperture It is larger, it is suitable for the preparation of catalyst carrier and catalyst.

Claims (4)

  1. A kind of 1. method that boehmite is prepared with FCC dead catalyst, it is characterised in that using FCC dead catalyst as raw material, warp Boehmite is made in the processes such as peracid treatment, filtration washing, removal of impurities, plastic, aging, filtration washing, drying, crushing, specifically Step is：
    A, FCC dead catalyst is added in acid solution, after stirring and evenly mixing, 1-8 h is reacted at 50-90 DEG C, are filtered afterwards Washing, filtrate is collected, obtains acid reaction liquid；
    B, the acid reaction liquid for obtaining step A, alkaline solution is added, fully after reaction, filtration washing, it is meta-aluminic acid to obtain filtrate Salting liquid；
    C, the filtrate that step B is obtained is mixed with aluminum salt solution, regulation system pH=7.5-12, under stirring, 60-100 DEG C aging 2-12 h, obtain reaction product；
    D, the reaction product for obtaining step C filters washing, is crushed after filtration cakes torrefaction, and boehmite is made.
  2. 2. the method as described in claim 1, it is characterised in that in described step A, acid solution be hydrochloric acid, sulfuric acid, nitric acid, At least one of formic acid and acetic acid, the addition of acidic materials are used for it with aoxidizing the theoretical of reactive aluminum in FCC dead catalyst The 120-200 % of amount, liquid-solid ratio are 3-10 L/kg.
  3. 3. the method as described in claim 1, it is characterised in that in described step B, alkaline solution is sodium hydroxide, hydroxide At least one of potassium, ammoniacal liquor, the addition of alkaline matter is its theoretical amount reacted with aluminium salt in acid reaction liquid 150-200%。
  4. 4. the method as described in claim 1, it is characterised in that in described step C, aluminium salt Al2(SO4)3、Al2(NO3)3、 AlCl3In any one.
CN201710340688.1A 2017-05-16 2017-05-16 A kind of preparation method of boehmite Pending CN107352565A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108751241A (en) * 2018-07-31 2018-11-06 菏泽华立新材料有限公司 A kind of alkali treatment method and its processing unit of aluminium isopropoxide dead catalyst
CN113582212A (en) * 2021-07-16 2021-11-02 上海簇睿低碳能源技术有限公司 Preparation method of pseudo-boehmite for adhesive
CN115920961A (en) * 2021-08-10 2023-04-07 中国石油天然气股份有限公司 Preparation method of silicon-containing pseudo-boehmite slurry
CN115920961B (en) * 2021-08-10 2024-05-28 中国石油天然气股份有限公司 Preparation method of silicon-containing pseudo-boehmite slurry

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108751241A (en) * 2018-07-31 2018-11-06 菏泽华立新材料有限公司 A kind of alkali treatment method and its processing unit of aluminium isopropoxide dead catalyst
CN113582212A (en) * 2021-07-16 2021-11-02 上海簇睿低碳能源技术有限公司 Preparation method of pseudo-boehmite for adhesive
CN115920961A (en) * 2021-08-10 2023-04-07 中国石油天然气股份有限公司 Preparation method of silicon-containing pseudo-boehmite slurry
CN115920961B (en) * 2021-08-10 2024-05-28 中国石油天然气股份有限公司 Preparation method of silicon-containing pseudo-boehmite slurry

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