CN103172084B - Solid phase preparation method of aluminosilicophosphate eutectic molecular sieve - Google Patents

Solid phase preparation method of aluminosilicophosphate eutectic molecular sieve Download PDF

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CN103172084B
CN103172084B CN201310124765.1A CN201310124765A CN103172084B CN 103172084 B CN103172084 B CN 103172084B CN 201310124765 A CN201310124765 A CN 201310124765A CN 103172084 B CN103172084 B CN 103172084B
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molecular sieve
crystallization
aluminosilicophosphate
aqueous solution
steam
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CN103172084A (en
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狄春雨
李晓峰
王晋梅
梁光华
王龙
窦涛
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CHIA TAI ENERGY MATERIALS (DALIAN) Co.,Ltd.
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Taiyuan Dacheng Huanneng Chemical Technology Co Ltd
Taiyuan University of Technology
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Abstract

The invention belongs to the technical field of the preparation of aluminosilicophosphate and in particular relates to a solid phase preparation method of an aluminosilicophosphate eutectic molecular sieve. The invention aims at solving the technical problem of providing a method for quickly preparing an aluminosilicophosphate eutectic molecular sieve in situ by adopting a solid phase method. According to the technical scheme, the solid phase preparation method comprises the following steps of: quickly mixing and stirring a silicon source, an aluminium source, a phosphorus source and water until gel is formed; drying the gel at a certain temperature, crushing the dried gel into small pieces and placing the small pieces into a reaction kettle; filling the mixture of a volatile template and water in a steam generator, and sealing the whole reaction device; opening a throttle valve of the steam generator, carrying out steam crystallization for a certain period of time at a certain temperature, so that the dried gel is converted into the aluminosilicophosphate eutectic molecular sieve; and after crystallization is finished, washing, drying and roasting the aluminosilicophosphate eutectic molecular sieve to obtain the finished product, and recycling an organic template in the steam generator. By adopting the solid phase preparation provided by the invention, the aluminosilicophosphate eutectic molecular sieve can be quickly prepared.

Description

A kind of method for preparing solid phase of aluminosilicophosphate eutectic molecular sieve
Technical field
The invention belongs to silicoaluminophosphamolecular molecular sieve preparing technical field, be specifically related to a kind of method for preparing solid phase of aluminosilicophosphate eutectic molecular sieve.
Background technology
Ethene and propylene are important Organic Chemicals, and along with the development of modern industrial society, its demand is increasing.The source of ethene and propylene is mainly by the catalytic pyrolysis of petroleum naphtha, solar oil etc. traditionally.But in recent years, along with the minimizing of oil production rate, its price soars rapidly, therefore make the cost producing low-carbon alkene more and more higher, this just needs people to develop the olefin production novel process of Non oil-based route, wherein, coal-based methyl alcohol processed again alkene processed is hopeful the revolutionary technology that petroleum replacing route produces low-carbon alkene most, and the key of this technology is catalyzer, up to the present, the catalyzer being applied to methanol-to-olefins reaction process is best with SAPO-34 molecular sieve catalyst performance.Therefore, the preparation of SAPO-34 molecular sieve and study on the modification are just become very meaningful.
US4440871 and US5279810 patent describes the preparation method of multiple phosphorus containing molecular sieve, these two sections of patents illustrate and adopt silicon source, aluminium source, phosphorus source and organic formwork agent to produce multiple SAPO molecular sieve, particularly including having the SAPO-34 molecular sieve of CHA skeleton structure and having the preparation of SAPO-18 molecular sieve of AEI skeleton structure.
US6334994 patent discloses a kind of silicoaluminophosphamolecular molecular sieve being referred to as RUW-19 and preparation method thereof, and it is reported that it is AEI/CHA eutectic composition, the catalyzer as methanol-to-olefins (MTO) has very high catalytic activity.
US Patent No. 2005/0233895 discloses a kind of two kinds of coexisting phase silicoaluminophosphamolecular molecular sieves containing AEI framework type material and CHA framework type material equally, by measuring the x-ray diffraction pattern of molecular sieve roasting sample, the ratio analyzing the AEI/CHA measuring described coexisting phase according to DIFFaX is about 5/95 to 40/60.
In addition, Dalian Inst of Chemicophysics, Chinese Academy of Sciences patent CN101450806A equally also reports AEI/CHA eutectic molecular sieve as MTO catalysts and synthetic method thereof.
More than have the silicoaluminophosphamolecular molecular sieve of AEI and CHA eutectic structure, its preparation method all adopts traditional hydrothermal synthesis method, and this method synthesis cycle is long, and organic amine template recycle difficulty is large; And utilize solid phase in situ conversion process to prepare eutectic molecular sieve to have not been reported.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, and technical problem to be solved is to provide a kind of method that solid phase method original position prepares aluminosilicophosphate eutectic molecular sieve fast.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of method for preparing solid phase of aluminosilicophosphate eutectic molecular sieve, comprises the following steps:
The first step, prepares gel: by silicon source, aluminium source, phosphorus source and water mixing rapid stirring until form gel;
Second step, prepares dry glue: dried at a certain temperature by above-mentioned gel, be broken into the dry glue of fritter and be placed in reaction unit;
3rd step, filling template: by template R 1and R 2r is mixed to get respectively with water 1the aqueous solution and R 2the aqueous solution, by R 1the aqueous solution and R 2the aqueous solution is respectively charged into reaction unit, and seals whole reaction unit;
4th step, crystallization: heat R respectively 1the aqueous solution and R 2the steam that the aqueous solution produces with template carries out steam crystallization to described dry glue;
5th step, crystallization terminates, and obtains aluminosilicophosphate eutectic molecular sieve, the organic formwork agent simultaneously in recovered steam producer.
A method for preparing solid phase for aluminosilicophosphate eutectic molecular sieve, described 4th step crystallization is for first to heat R 1the aqueous solution produces with template R 1steam steam crystallization is carried out to described dry glue, be then switched to R 2aqueous solution heating produces with template R 2steam proceed steam crystallization, all the other steps are the same.
A method for preparing solid phase for aluminosilicophosphate eutectic molecular sieve, described 4th step crystallization is for first to heat R 2the aqueous solution produces with template R 2steam steam crystallization is carried out to described dry glue, be then switched to R 1aqueous solution heating produces with template R 1steam proceed steam crystallization, all the other steps are the same.
The mol ratio in described silicon source, aluminium source, phosphorus source is SiO 2: Al 2o 3: P 2o 5=0.2 ~ 1.0:0.5 ~ 1.5:0.5 ~ 1.5; Described R 1the concentration of the aqueous solution is 7mol/L-83mol/L, R 2the concentration of the aqueous solution is 1.5mol/L-55.5mol/L.
Described silicon source is silicon sol, active silica, positive silicon ester or water glass, described aluminium source is activated alumina, pseudo-boehmite, aluminum alkoxide, aluminum isopropylate, aluminium salt, aluminate or Alumina gel, and described phosphorus source is ortho-phosphoric acid, phosphorous acid, phosphoric acid salt, Organophosphorous compounds or phosphorous oxides.
Described template R 1for diethylamine, triethylamine, morpholine, piperidines, Isopropylamine, dipropyl amine, described template R 2for DIPEA.
The crystallization temperature of described 4th step crystallization is 150 ~ 200 DEG C, uses R 1the time that the aqueous solution carries out steam crystallization is 2 ~ 12 hours, uses R 2the time that the aqueous solution carries out steam crystallization is 1 ~ 6 hour.
Described aluminosilicophosphate eutectic molecular sieve is AEI/CHA Eutectic Silicon in Al-Si Cast Alloys aluminophosphate molecular sieve, and the content of AEI crystallization is 1 ~ 10%.
In described AEI/CHA Eutectic Silicon in Al-Si Cast Alloys aluminophosphate molecular sieve, the more excellent content of AEI crystallization is 1 ~ 5%.
Compared with prior art the present invention has following beneficial effect.
1, the product of method needs tens of and even up to a hundred hours ability synthesis needs of silicoaluminophosphamolecular molecular sieve is originally prepared, the present invention adopts solid phase in-situ method to prepare the silicoaluminophosphamolecular molecular sieve with AEI/CHA eutectic structure, shorten the crystallization time of molecular sieve greatly, the longest generated time can not more than 20 hours.
2, method of the present invention is adopted first raw material to be prepared into the dry glue of solid phase, then template steam is adopted to carry out in-situ crystallization to synthesize the silicoaluminophosphamolecular molecular sieve of AEI/CHA eutectic structure to the dry glue of solid phase, owing to being employing solid phase in-situ synthesis, raw material is without any waste, after crystallization terminates, dry glue changes aluminosilicophosphate eutectic molecular sieve completely into, and therefore productive rate can reach 100%, and can not cause the waste of raw material.
3, adopt method of the present invention to synthesize the silicoaluminophosphamolecular molecular sieve of AEI/CHA eutectic structure, the content of AEI crystal can be controlled preferably in the scope needed.
4, adopt method synthesis of molecular sieve of the present invention, molecular sieve is separated with template liquid, eliminates numerous and diverse separating step.
5, method of the present invention can be good at realizing the recovery of template and recycles, and reduce the consumption of template, conservation, also can not cause environmental pollution.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described.
Fig. 1 is the product sample scanning electron microscope (SEM) photograph (SEM) of the embodiment of the present invention 1.
Embodiment
Embodiment 1
The first step, prepares gel: by 4.2g silicon sol (containing SiO 225wt%), pseudo-boehmite (the content Al of 9.0g 2o 365.5%) and the phosphoric acid of 13.6g (containing H 3pO 485wt%) add successively in 20g water, rapid stirring is until form gel;
Second step, prepares dry glue: gel is obtained dry glue and broken frustillatum in dry 1 day in 60 DEG C of baking ovens, puts into crystallization device;
3rd step, filling template: respectively by the N of the triethylamine of 20.5g and 8g deionized water and 4.5g, N-diisopropylethylamine and 5g deionized water are mixed to get the template aqueous solution, load the gained template aqueous solution into reaction unit respectively, seal whole reaction unit;
4th step, crystallization: carry out steam crystallization at 170 DEG C, the steam that first heating triethylamine aqueous solution produces with triethylamine carries out steam crystallization 12 hours to described dry glue, then be switched to N, the steam that the heating of the N-diisopropylethylamine aqueous solution produces with DIPEA proceeds steam crystallization 6 hours;
5th step, crystallization terminates, and obtains aluminosilicophosphate eutectic molecular sieve, the organic formwork agent simultaneously in recovered steam producer.
In the present embodiment gained AEI/CHA eutectic sample, AEI crystalline content accounts for the scanning electron microscope of about 4%, gained AEI/CHA overall eutectic sample as shown in Figure 1.
Embodiment 2
The first step, prepares gel: by 4.2g silicon sol (containing SiO 225wt%), pseudo-boehmite (the content Al of 8.3g 2o 365.5%) and the phosphoric acid of 12.5g (containing H 3pO 485wt%) add successively in 30g water, rapid stirring is until form gel;
Second step, prepares dry glue: gel is obtained dry glue and broken frustillatum in dry 1 day in 70 DEG C of baking ovens, puts into crystallization device;
3rd step, filling template: respectively by the N of the triethylamine of 20.5g and 10g deionized water and 5.6g, N-diisopropylethylamine and 5g deionized water are mixed to get the template aqueous solution, load the gained template aqueous solution into reaction unit respectively, seal whole reaction unit;
4th step, crystallization: carry out steam crystallization at 180 DEG C, first heat N, the N-diisopropylethylamine aqueous solution produces with N, the steam of N-diisopropylethylamine carries out steam crystallization 3 hours to described dry glue, and the steam be then switched to triethylamine aqueous solution heating produces with triethylamine proceeds steam crystallization 6 hours;
5th step, crystallization terminates, and obtains aluminosilicophosphate eutectic molecular sieve, the organic formwork agent simultaneously in recovered steam producer.
In the present embodiment gained AEI/CHA eutectic sample, AEI crystalline content accounts for overall about 8%.
Embodiment 3
The first step, prepares gel: by 4.8g silicon sol (containing SiO 225wt%), pseudo-boehmite (the content Al of 9.0g 2o 365.5%) and the phosphoric acid of 15.6g (containing H 3pO 485wt%) add successively in 30g water, rapid stirring is until form gel;
Second step, prepares dry glue: gel is obtained dry glue and broken frustillatum in dry 1 day in 70 DEG C of baking ovens, puts into crystallization device;
3rd step, filling template: respectively by the N of the diethylamine of 26.5g and 15g deionized water and 5.8g, N-diisopropylethylamine and 8g deionized water are mixed to get the template aqueous solution, load the gained template aqueous solution into reaction unit respectively, seal whole reaction unit;
4th step, crystallization: carry out steam crystallization at 170 DEG C, the steam that first heating diethylamine aqueous solution produces with diethylamine carries out steam crystallization 10 hours to described dry glue, then be switched to N, the steam that the heating of the N-diisopropylethylamine aqueous solution produces with DIPEA proceeds steam crystallization 3 hours;
5th step, crystallization terminates, and obtains aluminosilicophosphate eutectic molecular sieve, the organic formwork agent simultaneously in recovered steam producer.
In the present embodiment gained AEI/CHA eutectic sample, AEI crystalline content accounts for overall about 1.1%.
Embodiment 4
The first step, prepares gel: by 4.8g silicon sol (containing SiO 225wt%), pseudo-boehmite (the content Al of 9.6g 2o 365.5%) and the phosphoric acid of 15.6g (containing H 3pO 485wt%) add successively in 30g water, rapid stirring is until form gel;
Second step, prepares dry glue: gel is obtained dry glue and broken frustillatum in dry 1 day in 55 DEG C of baking ovens, puts into crystallization device;
3rd step, filling template: respectively by the N of the morpholine of 32.8g and 10g deionized water and 5.8g, N-diisopropylethylamine and 6g deionized water are mixed to get the template aqueous solution, load the gained template aqueous solution into reaction unit respectively, seal whole reaction unit;
4th step, crystallization: carry out steam crystallization at 175 DEG C, the steam that first the heating morpholine aqueous solution produces with morpholine carries out steam crystallization 8 hours to described dry glue, then be switched to N, the steam that the heating of the N-diisopropylethylamine aqueous solution produces with DIPEA proceeds steam crystallization 2 hours;
5th step, crystallization terminates, and obtains aluminosilicophosphate eutectic molecular sieve, the organic formwork agent simultaneously in recovered steam producer.
In the present embodiment gained AEI/CHA eutectic sample, AEI crystalline content accounts for overall about 3%.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, above-mentioned embodiment of the present invention all can only be thought explanation of the present invention and can not limit invention, claims indicate scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, all should think to be included in the scope of claims.

Claims (8)

1. a method for preparing solid phase for aluminosilicophosphate eutectic molecular sieve, is characterized in that comprising the following steps:
The first step, prepares gel: by silicon source, aluminium source, phosphorus source and water mixing rapid stirring until form gel;
Second step, prepares dry glue: dried at a certain temperature by above-mentioned gel, be broken into the dry glue of fritter and be placed in reaction unit;
3rd step, filling template: by template R 1and R 2r is mixed to get respectively with water 1the aqueous solution and R 2the aqueous solution, by R 1the aqueous solution and R 2the aqueous solution is respectively charged into reaction unit, and seals whole reaction unit;
4th step, crystallization: heat R respectively 1the aqueous solution and R 2the steam that the aqueous solution produces with template carries out steam crystallization to described dry glue;
5th step, crystallization terminates, and obtains aluminosilicophosphate eutectic molecular sieve, the organic formwork agent simultaneously in recovered steam producer;
Described template R 1for the one in diethylamine, triethylamine, morpholine, piperidines, Isopropylamine, dipropyl amine, described template R 2for DIPEA.
2. the method for preparing solid phase of a kind of aluminosilicophosphate eutectic molecular sieve according to claim 1, is characterized in that described 4th step crystallization is for first to heat R 1the aqueous solution produces with template R 1steam steam crystallization is carried out to described dry glue, be then switched to R 2aqueous solution heating produces with template R 2steam proceed steam crystallization.
3. the method for preparing solid phase of a kind of aluminosilicophosphate eutectic molecular sieve according to claim 1, is characterized in that described 4th step crystallization is for first to heat R 2the aqueous solution produces with template R 2steam steam crystallization is carried out to described dry glue, be then switched to R 1aqueous solution heating produces with template R 1steam proceed steam crystallization.
4., according to the method for preparing solid phase of any described a kind of aluminosilicophosphate eutectic molecular sieve of claim 1-3, it is characterized in that: the mol ratio in described silicon source, aluminium source, phosphorus source is SiO 2: Al 2o 3: P 2o 5=0.2 ~ 1.0:0.5 ~ 1.5:0.5 ~ 1.5; Described R 1the concentration of the aqueous solution is 7mol/L-83mol/L, R 2the concentration of the aqueous solution is 1.5mol/L-55.5mol/L.
5. according to the method for preparing solid phase of any described a kind of aluminosilicophosphate eutectic molecular sieve of claim 1-3, it is characterized in that: described silicon source is silicon sol, active silica, positive silicon ester or water glass, described aluminium source is activated alumina, pseudo-boehmite, aluminum alkoxide, aluminum isopropylate, aluminium salt, aluminate or Alumina gel, and described phosphorus source is ortho-phosphoric acid, phosphorous acid, phosphoric acid salt, Organophosphorous compounds or phosphorous oxides.
6., according to the method for preparing solid phase of any described a kind of aluminosilicophosphate eutectic molecular sieve of claim 1-3, it is characterized in that the crystallization temperature of described 4th step crystallization is 150 ~ 200 DEG C, use R 1the time that the aqueous solution carries out steam crystallization is 2 ~ 12 hours, uses R 2the time that the aqueous solution carries out steam crystallization is 1 ~ 6 hour.
7., according to the method for preparing solid phase of any described a kind of aluminosilicophosphate eutectic molecular sieve of claim 1-3, it is characterized in that: described aluminosilicophosphate eutectic molecular sieve is AEI/CHA Eutectic Silicon in Al-Si Cast Alloys aluminophosphate molecular sieve, and the content of AEI crystallization is 1 ~ 10%.
8. the method for preparing solid phase of a kind of aluminosilicophosphate eutectic molecular sieve according to claim 7, is characterized in that: in described AEI/CHA Eutectic Silicon in Al-Si Cast Alloys aluminophosphate molecular sieve, the content of AEI crystallization is 1 ~ 5%.
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Publication number Priority date Publication date Assignee Title
CN104556091B (en) * 2013-10-25 2016-05-25 中国石油化工股份有限公司 A kind of preparation method of SAPO-34 molecular sieve
CN104549483B (en) * 2013-10-28 2017-07-14 中国石油化工股份有限公司 Composite molecular screens of binder free SAPO 34/ZSM 5 and preparation method thereof
CN104760970A (en) * 2014-01-02 2015-07-08 上海复榆新材料科技有限公司 Method for synthesizing zeolite molecular sieve or SAPO molecular sieve, and apparatus thereof
CN105174286B (en) * 2015-08-17 2017-12-22 久泰能源科技有限公司 A kind of preparation method of the eutectic molecular sieves of AEI/CHA at high proportion
CN107915233B (en) * 2016-10-11 2019-11-08 中国石油化工股份有限公司 A kind of synthetic method of AEN structure aluminium silicophosphate molecular sieve and the application of the AEN structure aluminium silicophosphate molecular sieve
CN113277531A (en) * 2021-07-14 2021-08-20 中国矿业大学 Method for preparing small-crystal-grain SAPO-34 molecular sieve
CN114014337B (en) * 2022-01-05 2022-03-15 中汽研（天津）汽车工程研究院有限公司 AEI-CHA intergrowth molecular sieve and catalyst thereof
CN115159540B (en) * 2022-07-10 2024-04-30 苏州科技大学 Method for preparing molecular sieve and molecular sieve membrane by taking template agent as seed crystal
CN117023604B (en) * 2023-10-09 2024-01-02 中汽研汽车检验中心（天津）有限公司 Chabazite structure molecular sieve, catalyst, synthesis method and application thereof

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CN101125665A (en) * 2007-08-08 2008-02-20 华陆工程科技有限责任公司 Method for preparing SAPO-34 molecular sieve by liquid phase crystallization method
CN101428819A (en) * 2007-11-09 2009-05-13 汉能科技有限公司 Process for producing SAPO-5 molecular sieve

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