CN101817539A - Method for synthesizing A type molecular sieve by adopting attapulgite clay - Google Patents
Method for synthesizing A type molecular sieve by adopting attapulgite clay Download PDFInfo
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- CN101817539A CN101817539A CN200910021715A CN200910021715A CN101817539A CN 101817539 A CN101817539 A CN 101817539A CN 200910021715 A CN200910021715 A CN 200910021715A CN 200910021715 A CN200910021715 A CN 200910021715A CN 101817539 A CN101817539 A CN 101817539A
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- attapulgite clay
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- molecular sieve
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- 239000004927 clay Substances 0.000 title claims abstract description 33
- 229960000892 attapulgite Drugs 0.000 title claims abstract description 32
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 32
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 23
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 10
- 230000002194 synthesizing effect Effects 0.000 title abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 15
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 14
- 239000012265 solid product Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005352 clarification Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract 1
- 238000002242 deionisation method Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- CRPOUZQWHJYTMS-UHFFFAOYSA-N dialuminum;magnesium;disilicate Chemical compound [Mg+2].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] CRPOUZQWHJYTMS-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
采用凹凸棒石粘土合成A型分子筛的方法，选用或含铁在5％以下的凹凸棒石粘土，按摩尔比Na2O∶Al2O3∶SiO2∶H2O为3∶1∶2∶185选配上述凹凸棒石粘土，将其加入到4mol/L的NaOH溶液中，将溶液均分置于两个容器中，分别标为1号容器、2号容器；将含铁量在5％以下的凹凸棒粘土装入1号容器中，在80～90℃的温度下匀速搅拌1小时；在2号容器中加入铝酸钠溶解至澄清，然后快速倒入1号容器中，在30℃～40℃温度下搅拌30分钟，形成凝胶，置于烘箱中，进行密封，然后在90～100℃的温度下晶化3.5小时，将结晶固体产物通过过滤使固液分离，用去离子水将固体产物洗涤到pH小于9，在80～110℃温度下进行干燥，时间超过12小时，即得A型分子筛。The method of synthesizing type A molecular sieve by using attapulgite clay is selected or attapulgite clay with iron content below 5%, and the molar ratio of Na 2 O:Al 2 O 3 :SiO 2 :H 2 O is 3:1:2 : 185 selects above-mentioned attapulgite clay, joins it in the NaOH solution of 4mol/L, the solution is placed in two containers equally, is marked as No. 1 container, No. 2 container respectively; Attapulgite clay below % was put into No. 1 container, and stirred at a constant speed for 1 hour at a temperature of 80-90°C; in No. 2 container, sodium aluminate was added to dissolve until clear, and then quickly poured into No. Stir at ℃～40℃ for 30 minutes to form a gel, put it in an oven, seal it, and then crystallize it at a temperature of 90～100℃ for 3.5 hours, filter the crystalline solid product to separate the solid and liquid, and use deionization The solid product is washed with water until the pH is less than 9, and dried at a temperature of 80-110° C. for more than 12 hours to obtain a type A molecular sieve.
Description
Technical field
The present invention relates to adopt attapulgite clay to prepare the method for A type molecular sieve.
Background technology
China be the main attapulgite clay in the world main contain state and producing country, its main component silico-aluminate.Molecular sieve is a kind of silico-aluminate of crystal form, and its spacial framework is by silicon-oxy tetrahedron unit [SiO
4] and aluminum-oxygen tetrahedron [AlO
4] unit is staggered and forms, its structure is very similar to NaCl, and its chemical group journey general formula is Na
2O: Al
2O
3: 2SiO
2: 5H
2O belongs to isometric system.Because its uniform pore size and big area exist large quantity of moisture and positively charged ion in structure, this construction features make molecular sieve have absorption, catalysis and the ion-exchange three big characteristics of selection.Therefore be widely used in industries such as oil, chemistry, metallurgy.The method of producing at present 4A type molecular sieve has chemical feedstocks preparation method (being complete synthesizing process) and with clay preparation method (being semi-synthesis method).People such as Hewell at first utilize kaolin to synthesize the 4A molecular sieve, be the extensive attention that the method for the synthetic 4A molecular sieve of raw material has been subjected to Chinese scholars subsequently with the natural mineral, successively utilize crude substance such as diatomite, perlite, bauxite, wilkinite to successfully synthesize the 4A molecular sieve, but domestic do not see attapulgite clay mining in the study on the synthesis of 4A molecular sieve.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts the synthetic A type molecular sieve of attapulgite clay.
The present invention is the method that adopts the synthetic A type molecular sieve of attapulgite clay, the steps include:
(1) select for use or iron content at the attapulgite clay below 5%, silicone content is 40～70% in its attapulgite clay ore deposit, the content of aluminium is 6～18%; Selecting content for use is sodium aluminate more than 95%, and content is the sodium hydroxide more than 95%;
(2) Na in molar ratio
2O: Al
2O
3: SiO
2: H
2O is 3: 1: 2: 185 apolegamys join above-mentioned attapulgite clay in the NaOH solution of 4mol/L with it, stir 10～20 minutes to all dissolving, and solution all is placed in two containers, are denoted as No. 1 container, No. 2 containers;
(3) with iron-holder in the attapulgite clay below 5% is packed No. 1 container into, under 80～90 ℃ temperature, at the uniform velocity stirred 1 hour;
(4) in No. 2 containers, add the sodium aluminate dissolving to clarification, pour into fast then in No. 1 container, under 30 ℃～40 ℃ temperature, stirred 30 minutes, form gel, place baking oven or thermostatical oil bath, seal, then crystallization 3.5 hours under 90～100 ℃ temperature, crystallization finishes, and is cooled to room temperature;
(5) the crystalline solid product is made solid-liquid separation by filtration, with deionized water solid product is washed PH less than 9, put into baking oven and carry out drying under 80～110 ℃ of temperature, the time surpasses 12 hours, promptly gets A type molecular sieve.
Perhaps:
(1) iron-holder being pulverized at the attapulgite clay below 5%, crossed 120 mesh sieves, is to mix at 1: 1.2 with yellow soda ash with mass ratio, puts into high-temperature roasting device and carry out roasting under 800 ℃ temperature, time remaining 1 hour;
(2) sodium aluminate is dissolved in water, under 30 ℃～40 ℃ temperature, stirred 30 minutes;
(3) material after the roasting is packed in the container, add sodium aluminate solution, under 60 ℃ of temperature, stir, form gel, place baking oven or thermostatical oil bath, seal, be warming up to 90 ℃～100 ℃ then and carry out crystallization, time remaining 6～8 hours;
(4) after reaction finishes, the crystalline solid product being made solid-liquid separation by filtration, is till 7～8 with distilled water wash to pH, puts into baking oven and carry out drying under 80～110 ℃ of temperature, promptly gets A type molecular sieve.
Embodiment
Be explanation specific embodiments of the invention into below, it is synthetic and make it to be converted into amorphous substance with high-temperature roasting to be divided into hydro-thermal, carries out the synthetic two portions of hydro-thermal again.
Embodiment 1-1:
(1) select for use or iron content at the attapulgite clay below 5%;
(2) Na in molar ratio
2O: Al
2O
3: SiO
2: H
2O is 3: 1: 2: the above-mentioned attapulgite clay of 185 apolegamys, it is joined in the NaOH solution of 3L4mol/L, and stirs 10～20 minutes to all dissolving, solution all is placed in two containers, be denoted as No. 1 container, No. 2 containers;
(3) with the 125g iron-holder in the attapulgite clay below 5% is packed No. 1 container into, under 80～90 ℃ temperature, at the uniform velocity stirred 1 hour;
(4) in No. 2 containers, add the dissolving of 117g sodium aluminate to clarification, pour into fast then in No. 1 container, under 30 ℃ of temperature, stirred 30 minutes, form gel, place baking oven or thermostatical oil bath, seal, crystallization 3.5 hours under 90 ℃ temperature then, crystallization finishes, and is cooled to room temperature;
(5) the crystalline solid product is made solid-liquid separation by filtration, with deionized water solid product is washed PH less than 9, put into baking oven and carry out drying under 80 ℃ of temperature, the time surpasses 12 hours, promptly gets A type molecular sieve.
Embodiment 1-2:
(1) select for use or iron content at the attapulgite clay below 5%, Na in molar ratio
2O: Al
2O
3: SiO
2: H
2O is 3: 1: 2: the above-mentioned attapulgite clay of 185 apolegamys, it is joined in the NaOH solution of 1.5L4mol/L, and stirs 10～20 minutes to all dissolving, solution all is placed in two containers, be denoted as No. 1 container, No. 2 containers;
(2) with the 125g iron-holder in the attapulgite clay below 5% is packed No. 1 container into, under 90 ℃ temperature, at the uniform velocity stirred 1 hour;
(3) in No. 2 containers, add 58.5g and separate, pour into fast then in No. 1 container, under 40 ℃ of temperature, stirred 30 minutes to clarification, form gel, place baking oven or thermostatical oil bath, seal, crystallization 3.5 hours under 100 ℃ temperature then, crystallization finishes, and is cooled to room temperature;
(4) the crystalline solid product is made solid-liquid separation by filtration, with deionized water solid product is washed PH less than 9, put into baking oven and carry out drying under 110 ℃ of temperature, the time surpasses 12 hours, promptly gets A type molecular sieve.
Embodiment 2-1:
(1) select for use or iron content at the attapulgite clay below 5%, Na in molar ratio
2O: Al
2O
3: SiO
2: H
2O is 3: 1: 2: the above-mentioned attapulgite clay of 185 apolegamys, and concrete component is: contain Si42.1%; Al6.2%; Ca35%; Fe5.68% with its pulverizing, crosses 120 mesh sieves, and 200 gram attapulgite clays are mixed with 240 gram yellow soda ash, puts into muffle furnace and carry out roasting under 800 ℃ temperature, time remaining 1 hour;
(2) sodium aluminate with 300 grams dissolves in water, stirs 30 minutes under 40 ℃ temperature;
(3) material after the roasting is packed in the container, add sodium aluminate solution, under 60 ℃ temperature, stir, form gel, place baking oven, seal, be warming up to then and carry out crystallization under 90 ℃, time remaining 6 hours;
(4) after reaction finishes, the crystalline solid product being made solid-liquid separation by filtration, is till 7 with distilled water wash to pH, puts into baking oven and carry out drying under 80 ℃ temperature, and the time promptly got A type molecular sieve above 12 hours.
Embodiment 2-2:
(1) select for use or iron content at the attapulgite clay below 5%, Na in molar ratio
2O: Al
2O
3: SiO
2: H
2O is 3: 1: 2: the above-mentioned attapulgite clay of 185 apolegamys, and concrete component is: contain Si 51.8%; Al 16.0%; Ca 1.585%; Fe 5.46%, with its pulverizing, crosses 120 orders, and 200 gram attapulgite clays are mixed with 240 gram yellow soda ash, puts into muffle furnace 800 ℃ of following roastings 1 hour.
(2) sodium aluminate with 162 grams dissolves in a spot of water, stirs 30 minutes down at 40 ℃;
(3) material after the roasting is packed in the container, adds the sodium aluminate solution after the dissolving, stirs under 60 ℃ temperature, forms gel, places the thermostatical oil bath, seals, and is warming up to then under 100 ℃ the temperature to carry out crystallization, time remaining 8 hours;
(4) after reaction finishes, the crystalline solid product being made solid-liquid separation by filtration, is till 8 with distilled water wash to pH, puts into baking oven and carry out drying under 110 ℃ temperature, and the time promptly got A type molecular sieve above 12 hours.
Claims (1)
1. adopt the method for the synthetic A type molecular sieve of attapulgite clay, the steps include:
(1) select for use or iron content at the attapulgite clay below 5%, silicone content is 40～70% in its attapulgite clay ore deposit, the content of aluminium is 6～18%; Selecting content for use is sodium aluminate more than 95%, and content is the sodium hydroxide more than 95%;
(2) Na in molar ratio
2O: Al
2O
3: SiO
2: H
2O is 3: 1: 2: the above-mentioned attapulgite clay of 185 apolegamys, it is joined in the NaOH solution of 4mol/L, and stirs 10～20 minutes to all dissolving, solution all is placed in two containers, be denoted as No. 1 container, No. 2 containers;
(3) with iron-holder in the attapulgite clay below 5% is packed No. 1 container into, under 80～90 ℃ temperature, at the uniform velocity stirred 1 hour;
(4) in No. 2 containers, add the sodium aluminate dissolving to clarification, pour into fast then in No. 1 container, under 30 ℃～40 ℃ temperature, stirred 30 minutes, form gel, place baking oven or thermostatical oil bath, seal, then crystallization 3.5 hours under 90～100 ℃ temperature, crystallization finishes, and is cooled to room temperature;
(5) the crystalline solid product is made solid-liquid separation by filtration, with deionized water solid product is washed PH less than 9, put into baking oven and carry out drying under 80～110 ℃ of temperature, the time surpasses 12 hours, promptly gets A type molecular sieve.
Perhaps:
(1) iron-holder being pulverized at the attapulgite clay below 5%, crossed 120 mesh sieves, is to mix at 1: 1.2 with yellow soda ash with mass ratio, puts into high-temperature roasting device and carry out roasting under 800 ℃ temperature, time remaining 1 hour;
(2) sodium aluminate is dissolved in water, under 30 ℃～40 ℃ temperature, stirred 30 minutes;
(3) material after the roasting is packed in the container, add sodium aluminate solution, under 60 ℃ of temperature, stir, form gel, place baking oven or thermostatical oil bath, seal, be warming up to 90 ℃～100 ℃ then and carry out crystallization, time remaining 6～8 hours;
(4) after reaction finishes, the crystalline solid product being made solid-liquid separation by filtration, is till 7～8 with distilled water wash to pH, puts into baking oven and carry out drying under 80～110 ℃ of temperature, promptly gets A type molecular sieve.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910021715A CN101817539A (en) | 2009-03-14 | 2009-03-14 | Method for synthesizing A type molecular sieve by adopting attapulgite clay |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910021715A CN101817539A (en) | 2009-03-14 | 2009-03-14 | Method for synthesizing A type molecular sieve by adopting attapulgite clay |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101817539A true CN101817539A (en) | 2010-09-01 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583431A (en) * | 2012-01-10 | 2012-07-18 | 兰州大学 | Method for preparing 4A molecular sieves by doping bentonite with attapulgite |
| CN103170304A (en) * | 2013-03-11 | 2013-06-26 | 常州大学 | Method for preparing 5A molecular sieve for straight-chain paraffin adsorption through adopting attapulgite |
| CN103738978A (en) * | 2014-01-13 | 2014-04-23 | 大连北地科技有限公司 | Method for preparing NaX-type zeolite molecular sieve pure phase by using clay |
| CN109665810A (en) * | 2019-02-13 | 2019-04-23 | 安徽峰可达科技股份有限公司 | A kind of molecular screen membrane supporter and preparation method thereof and molecular screen membrane |
-
2009
- 2009-03-14 CN CN200910021715A patent/CN101817539A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583431A (en) * | 2012-01-10 | 2012-07-18 | 兰州大学 | Method for preparing 4A molecular sieves by doping bentonite with attapulgite |
| CN103170304A (en) * | 2013-03-11 | 2013-06-26 | 常州大学 | Method for preparing 5A molecular sieve for straight-chain paraffin adsorption through adopting attapulgite |
| CN103738978A (en) * | 2014-01-13 | 2014-04-23 | 大连北地科技有限公司 | Method for preparing NaX-type zeolite molecular sieve pure phase by using clay |
| CN103738978B (en) * | 2014-01-13 | 2015-11-25 | 大连北地科技有限公司 | A kind of clay prepares the method for NaX type zeolite molecular sieve pure phase |
| CN109665810A (en) * | 2019-02-13 | 2019-04-23 | 安徽峰可达科技股份有限公司 | A kind of molecular screen membrane supporter and preparation method thereof and molecular screen membrane |
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Open date: 20100901 |