CN1087030A - The preparation of binder free 5A wax molecular sieve adsorbent - Google Patents
The preparation of binder free 5A wax molecular sieve adsorbent Download PDFInfo
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- CN1087030A CN1087030A CN 92111878 CN92111878A CN1087030A CN 1087030 A CN1087030 A CN 1087030A CN 92111878 CN92111878 CN 92111878 CN 92111878 A CN92111878 A CN 92111878A CN 1087030 A CN1087030 A CN 1087030A
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- molecular sieve
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 43
- 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 43
- 239000003463 adsorbent Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011230 binding agent Substances 0.000 title claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000004927 clay Substances 0.000 claims abstract description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 5
- 235000019890 Amylum Nutrition 0.000 claims abstract description 5
- 241000196324 Embryophyta Species 0.000 claims abstract description 5
- 229920002472 Starch Polymers 0.000 claims abstract description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000001110 calcium chloride Substances 0.000 claims abstract description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 4
- 238000005342 ion exchange Methods 0.000 claims abstract description 4
- 244000275012 Sesbania cannabina Species 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000013067 intermediate product Substances 0.000 claims 2
- 239000000047 product Substances 0.000 claims 1
- 238000003795 desorption Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 241000219782 Sesbania Species 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 108060003393 Granulin Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 235000011868 grain product Nutrition 0.000 description 1
- 102000017941 granulin Human genes 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- YIEDSISPYKQADU-UHFFFAOYSA-N n-acetyl-n-[2-methyl-4-[(2-methylphenyl)diazenyl]phenyl]acetamide Chemical compound C1=C(C)C(N(C(C)=O)C(=O)C)=CC=C1N=NC1=CC=CC=C1C YIEDSISPYKQADU-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
A kind of preparation method of binder free 5A wax molecular sieve absorption, be to adopt conventional synthetic 5A preparation of molecular sieve, add kaolin families clay and 0.2～2% sesbania powder in synthetic 4A molecular sieve process or after the crystal washing of synthetic back by crystal weight 15～35%, sodium cellulosate or other plant amylum moulding are handled and are carried out ion-exchange with calcium chloride and make through sodium hydroxide solution again.This technical process is simple, product mechanical strength height, and the speed of absorption, desorption n-alkane is fast, good hydrothermal stability.In addition, this product also can be used for preparing with air the high-efficiency adsorbent of oxygen rich gas.
Description
The invention provides a kind of preparation method of adsorbent of molecular sieve, specifically provided a kind of separation that is suitable for positive isoparaffin, can be used as a kind of 5A adsorbent of molecular sieve of good dewaxing adsorbent.
The particulate molecular sieve product can be prepared by diverse ways, uses the micro crystal powder of pure molecular sieve usually, adds binding agent (as the clay of kaolin families), and through extruding, processes such as spin make.The sieve particle that can prepare binder free with hot extrusion briquetting technique.Also can adopt and give system sieve and silica-sesquioxide particle and obtain through alkali treatment.No matter adopt which kind of preparation technology's particulate molecular sieve, its sieve particle inside all exists the hole of difformity and size.Being the crystal microcellular structure of molecular sieve itself, secondly is between the molecular sieve crystal, between molecular sieve crystal and the binding agent particle, and the hole that in forming process, forms between the binding agent particle, be referred to as second pore structure.The size of its size and shape and molecular sieve crystallite, the kind of binding agent and quantity, the thickness program of binding agent particle and the technical process of moulding etc. are relevant.General pore-size distribution is very wide, and these holes provide very little specific area, does not generally play a major role in absorption and catalytic action, and second pore structure all has very big influence to diffusion, mechanical performance and the heat endurance of granulin molecule sieve.The performance of adding the zeolite product of adhesive preparation by molecular screen primary powder is subjected to the combined influence of many factors, and the zeolite product of argillaceous binding agent mechanical strength is preferably often arranged, but its adsorption rate is slower usually.Grain products is carried out necessary processing can improve its absorption property.For example U.S. Pat 3,386, and 802 and US3,356,086 technology.Adopt the alumina silicate micelle of preparation 4A to handle, make it be converted into the 4A molecular sieve, handle 2 times, get 62% 5A molecular sieve of sodium exchange capacity with 10% calcium chloride solution at 100 ℃ with sodium metasilicate and aqueous slkali.U.S. Pat 3,394989 is carried and has been total to that to add a spot of molecular screen primary powder with clay be raw material, adopts to give moulding process and prepare molecular sieve, handles with alkali lye and improves product permeability structure.But its complicated operating process of above-mentioned technology, the high temperature resistance hydro-thermal, the speed of less stable, absorption, desorption n-alkane is slower.
The purpose of this invention is to provide a kind of mechanical strength height, have strong high temperature resistance hydrothermal stability and higher absorption, the 5A adsorbent of molecular sieve of desorption n-alkane, this adsorbent is specially adapted to the alkane dewaxing technique.
The process of the preparation binder free 5A wax molecular sieve that the present invention proposes is in synthetic 4A molecular sieve process or after the crystal washing, adding 15～35%(weight) kaolin families clay and 0.2～2%(are heavy) sesbania powder or sodium cellulosate moulding, in 450～600 ℃ of following roastings, with handling in 0.5～3.0N sodium hydrate aqueous solution, washing back product makes product with the exchange of 0.05～2.0M calcium chloride water after washing, the drying.
Binder free 5A wax molecular sieve preparation of adsorbent method provided by the invention, utilize the technology of conventional preparation 5A molecular sieve, it is characterized in that in synthetic 4A molecular sieve process or add by crystal 15～35%(heavy in synthetic crystal washing back) kaolin families clay and 0.2～2% sesbania powder, sodium cellulosate or other plant amylum moulding, and then under 400～600 ℃, carry out roasting, roasting time is no less than 1 hour, makes the 4A molecular sieve; Above-mentioned 4A molecular sieve available hydrogen aqueous solution of sodium oxide is handled, and carries out ion-exchange with calcium chloride water again after the washing, and the exchange afterproduct obtains adsorbent of the present invention through washing after the drying.When carrying out naoh treatment, 0.5～3.0N NaOH solution commonly used, ion-exchange is with 0.05～2.0M CaCl
2The aqueous solution gives to illustrate further to the technology of the present invention below by example.
Example 1 binder free 5A wax molecular sieve adsorbent preparation 1
Prepare 4A molecular sieve technology routinely and get a certain amount of sodium metasilicate, sodium aluminate and sodium hydroxide solution in mixed glue still, stir into even gel, amount by synthetic 4A molecular sieve, the addition of clay is 20%, the addition of sesbania powder is 0.5%, heats to 100～110 ℃ under stirring behind adding clay and the sesbania powder again and makes it to react synthetic 4A molecular sieve.Product is drained after filtration, moulding, dry in 500 ℃ of following roastings 3 hours, handles 2 hours with the 1.0N sodium hydroxide solution, and treatment temperature is 90～98 ℃ and obtains the 4A molecular sieve.It is 23.78%(weight that the 4A molecular sieve is recorded the water saturation adsorbance with the drier method of room temperature saturated nacl aqueous solution).
Example 2 adsorbents preparation 2
4A powder 160 grams are added 40 gram clays add sodium cellulosate 1 gram, add 300 milliliters in water, after stirring, filtration is drained, moulding, oven dry, 500 ℃ of following roastings 3 hours, the 4A molecular sieve of forming is dissolved in 90～95 ℃ of processing 6 hours with 0.6N NaOH, washing, drying, making 4A product adsorpting water quantity is that 23.89%(is heavy).
Example 3 adsorbents preparation 3
Get 80 gram 4A and add 20 gram clays and add 0.3 gram sesbania powder, add 300 ml waters mix after filtration drain, moulding, dry back is in 550 ℃ of roastings 3 hours, handles in 90～98 ℃ with the 1.5N sodium hydroxide solution and keeps 2 hours.The sample adsorpting water quantity is that 22.62%(is heavy).
Example 4 adsorbents preparation 4
Get 600 gram 4A powder and add 120 gram clays, add 3 gram sesbania powder, 1800 ml waters be mixed the back filter drain, moulding, drying, in 550 ℃ of roastings 3 hours, sample was handled 8 hours in 90～95 ℃ in 1.0NaH solution, the sample adsorpting water quantity is 23.82%.
Example 5 adsorbents preparation 5
To contain adding 40 gram clays and 0.5 gram sesbania powder in the 200 gram 4A products, the back that stirs is filtered and is drained, and moulding, drying in 500 ℃ of following roastings 3 hours, are used 2.0N NaOH solution-treated 2 hours.The sample adsorpting water quantity is that 22.69%(is heavy).
Example 6 adsorbents preparation 6
To contain 4A powder 160 gram and add 20 gram clays and add sodium cellulosate 1 gram, add 300 milliliters in water, after stirring, filter drain, moulding, oven dry, 500 ℃ of following roastings 3 hours, with sample with 0.5N NaOH solution-treated 12 hours.The sample water absorption capacity is that 23.67%(is heavy).
Preparation 7 of example 7 adsorbents and absorption property test
4A product with above-mentioned example 1,2,3,4,5 makes exchanges 6 hours with the 1N calcium chloride solution under 70～80 ℃, get the 5A zeolite product.This product absorption nC
0 10The hydrocarbon amount with separate O
2, N
2Gas retention tabulation 1.
The performance test of table 1 binder free 5A molecular sieve adsorption
(1) sample finds time to activate 3 hours at 550 ℃, and under 350 ℃, 0.7 in nC
0 10Pressure is measured adsorbance down.
(2) sample with one meter osmanthus, is down measured gas insulating value at 40 ℃ 550 ℃ of activation 2 hours.
By above-described embodiment, characteristics of the present invention are:
1, in synthetic A type molecular sieve process, add binding agent and sesbania powder, the method for other plant amylum or sodium cellulosate is prepared the 5A molecular sieve that does not contain Binder Properties, its mechanical strength height, not shedding, simplification preparation process;
2, this sample 5A molecular sieve has the high temperature resistance hydrothermal stability, and has improved absorption, and the speed of desorption n-alkane has reduced the sensitiveness to poisonous substance (pyridine);
3, add the sesbania powder in the preparation process, other plant amylum or sodium cellulosate have improved the pore structure of adsorbent.Adsorbent is accelerated the diffusion rate of hydro carbons.
4, this adsorbent has very weak acid centre, is 1/4 of present commercially available wax molecular sieve product acid amount;
5, this product is to O in the air
2, N
2The absorption retention, be respectively 6.05ml/g, 13.50ml/g can be used for the high-efficiency adsorbent with air preparation oxygen rich gas.
Claims (3)
1, a kind of synthetic 5A preparation of molecular sieve of routine that adopts prepares the method for binder free 5A wax molecular sieve absorption, it is characterized in that in the synthetic 4A molecular sieve process or after the crystal washing of synthetic back, adding kaolin families clay and 0.2～2% sesbania powder, sodium cellulosate or other plant amylum moulding, and then under 400～600 ℃, carry out roasting and make intermediate product 4A molecular sieve by crystal weight 15～35%.
2, in accordance with the method for claim 1, it is characterized in that made intermediate product 4A molecular sieve can handle with the sodium hydrate aqueous solution of 0.5～3.0N.
3, in accordance with the method for claim 1, it is characterized in that carrying out ion-exchange with 0.05～2.0M calcium chloride water again through the product after the naoh treatment makes 5A adsorbent of molecular sieve of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111878 CN1042021C (en) | 1992-11-17 | 1992-11-17 | Preparation of adhesive-free 5A dewaxing molecular sieve adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111878 CN1042021C (en) | 1992-11-17 | 1992-11-17 | Preparation of adhesive-free 5A dewaxing molecular sieve adsorbent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1087030A true CN1087030A (en) | 1994-05-25 |
| CN1042021C CN1042021C (en) | 1999-02-10 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92111878 Expired - Fee Related CN1042021C (en) | 1992-11-17 | 1992-11-17 | Preparation of adhesive-free 5A dewaxing molecular sieve adsorbent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1042021C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100471555C (en) * | 2005-05-25 | 2009-03-25 | 太原理工大学 | Preparation method of high adsorption capacity zeolite molecular sieve adsorbent |
| CN103028374A (en) * | 2012-12-28 | 2013-04-10 | 天津众智科技有限公司 | 5A molecular sieve with high adsorption rate |
| CN104628009A (en) * | 2015-02-11 | 2015-05-20 | 河南环宇分子筛有限公司 | Method for synthesizing 5A type dewaxing molecular sieve from bentonite |
| CN105749859A (en) * | 2014-12-17 | 2016-07-13 | 中国石油天然气股份有限公司 | Preparation method for methyl methacrylate deacidification adsorbent |
| CN111097367A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Adsorbent for adsorbing normal alkane and preparation method and application thereof |
| CN114682237A (en) * | 2020-12-31 | 2022-07-01 | 中国石油化工股份有限公司 | Preparation method of 5A molecular sieve adsorbent |
| CN115155519A (en) * | 2022-08-01 | 2022-10-11 | 中科洁力（福州）环保技术有限公司 | Preparation method of molecular sieve with strong adsorbability |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292831C (en) * | 2003-03-11 | 2007-01-03 | 中美合资上海锦中分子筛有限公司 | High-performance variable-pressure adsorption 5A molecular sieve and preparing method thereof |
-
1992
- 1992-11-17 CN CN 92111878 patent/CN1042021C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100471555C (en) * | 2005-05-25 | 2009-03-25 | 太原理工大学 | Preparation method of high adsorption capacity zeolite molecular sieve adsorbent |
| CN103028374A (en) * | 2012-12-28 | 2013-04-10 | 天津众智科技有限公司 | 5A molecular sieve with high adsorption rate |
| CN103028374B (en) * | 2012-12-28 | 2014-12-17 | 天津众智科技有限公司 | 5A molecular sieve with high adsorption rate |
| CN105749859A (en) * | 2014-12-17 | 2016-07-13 | 中国石油天然气股份有限公司 | Preparation method for methyl methacrylate deacidification adsorbent |
| CN105749859B (en) * | 2014-12-17 | 2018-05-04 | 中国石油天然气股份有限公司 | Preparation method for methyl methacrylate deacidification adsorbent |
| CN104628009A (en) * | 2015-02-11 | 2015-05-20 | 河南环宇分子筛有限公司 | Method for synthesizing 5A type dewaxing molecular sieve from bentonite |
| CN111097367A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Adsorbent for adsorbing normal alkane and preparation method and application thereof |
| CN114682237A (en) * | 2020-12-31 | 2022-07-01 | 中国石油化工股份有限公司 | Preparation method of 5A molecular sieve adsorbent |
| CN114682237B (en) * | 2020-12-31 | 2023-09-01 | 中国石油化工股份有限公司 | Preparation method of 5A molecular sieve adsorbent |
| CN115155519A (en) * | 2022-08-01 | 2022-10-11 | 中科洁力（福州）环保技术有限公司 | Preparation method of molecular sieve with strong adsorbability |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1042021C (en) | 1999-02-10 |
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