CN102491362A - Method for preparing cation exchange content W type zeolite molecular sieve - Google Patents
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- CN102491362A CN102491362A CN2011103837103A CN201110383710A CN102491362A CN 102491362 A CN102491362 A CN 102491362A CN 2011103837103 A CN2011103837103 A CN 2011103837103A CN 201110383710 A CN201110383710 A CN 201110383710A CN 102491362 A CN102491362 A CN 102491362A
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- molecular sieve
- type zeolite
- zeolite molecular
- ammonium
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 65
- 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 65
- 239000010457 zeolite Substances 0.000 title claims abstract description 61
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 60
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000005341 cation exchange Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000003868 ammonium compounds Chemical class 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 10
- -1 ammonium ions Chemical class 0.000 claims abstract description 8
- 150000001768 cations Chemical class 0.000 claims abstract 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract 8
- 238000002360 preparation method Methods 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 6
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000005695 Ammonium acetate Substances 0.000 claims description 4
- 229940043376 ammonium acetate Drugs 0.000 claims description 4
- 235000019257 ammonium acetate Nutrition 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical group [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910001416 lithium ion Chemical group 0.000 claims description 3
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical group [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 description 25
- 239000000243 solution Substances 0.000 description 23
- 125000002091 cationic group Chemical group 0.000 description 16
- 239000007787 solid Substances 0.000 description 11
- 239000007795 chemical reaction product Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 238000005342 ion exchange Methods 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 6
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 229910001414 potassium ion Inorganic materials 0.000 description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000001166 ammonium sulphate Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- JEWHCPOELGJVCB-UHFFFAOYSA-N aluminum;calcium;oxido-[oxido(oxo)silyl]oxy-oxosilane;potassium;sodium;tridecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.O.[Na].[Al].[K].[Ca].[O-][Si](=O)O[Si]([O-])=O JEWHCPOELGJVCB-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004899 motility Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910001743 phillipsite Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
一种制备阳离子交换容量W型沸石分子筛的方法，主要步骤为：A)将含有初始阳离子Ci形式的W型沸石分子筛与含有铵离子的水溶性铵化合物接触，得到的含铵离子的W型沸石分子筛中(NH4)2O/Al2O3≥0.8；B)将步骤A得到的含铵离子的W型沸石分子筛与含最终阳离子Cf的溶液接触，用至少一种所述阳离子取代铵离子，并从反应区除去挥发性氨，制得的产物中CfO/Al2O3≥0.7，(NH4)2O/Al2O3≤0.1；C)将步骤B得到的产物用含Cf的溶液洗涤，干燥，最终得到阳离子交换容量W型沸石分子筛。A method for preparing W-type zeolite molecular sieve with cation exchange capacity, the main steps are: A) contacting the W-type zeolite molecular sieve containing the initial cation Ci form with a water-soluble ammonium compound containing ammonium ions, and obtaining the W-type zeolite containing ammonium ions (NH 4 ) 2 O/Al 2 O 3 ≥ 0.8 in the zeolite molecular sieve; B) contacting the W-type zeolite molecular sieve containing ammonium ion obtained in step A with the solution containing the final cation Cf , and replacing it with at least one of the cations ammonium ions, and remove volatile ammonia from the reaction zone, C f O/Al 2 O 3 ≥ 0.7 in the obtained product, (NH 4 ) 2 O/Al 2 O 3 ≤ 0.1; C) the product obtained in step B Washing with a solution containing Cf and drying to finally obtain a W-type zeolite molecular sieve with cation exchange capacity.
Description
Technical field
The present invention relates to a kind of polynary cationic exchange and produce the method for high-cation exchange capacity W type molecular sieve; More particularly; Relate to through W type molecular sieve is at first formed the w-type zeolite molecular sieve that contains ammonium form with ammonium ion exchange; To contain the w-type zeolite molecular sieve and the target cationic source of ammonium form then, under the condition of evicting ammonia from the zone of action from, contact, produce the method for high-cation exchange capacity W type molecular sieve.
Background technology
W-type zeolite molecular sieve SiO
2/ Al
2O
3Ratio be 3.2-4.8, its positively charged ion is generally potassium ion, structural formula is generally 1.02K
2O:Al
2O
3: 3.65SiO
2: 5.1H
2O.The w-type zeolite molecular sieve belongs to phillipsite family, has a series of tetra-atomic rings, the long band of the bending that its limit forms, and the main channel is an octatomic ring, free aperture is 4.8A to the maximum.As stated, the positively charged ion of w-type zeolite is generally potassium ion, has useful function although contain the potassium w-type zeolite in many-sides such as industry and environmental protection fields, preferably they is carried out IX, with its absorption property of further enhancing.Conventional exchange step can be used for preparing many single cationic exchange zeolites economically; Yet; The conventional in all cases potassium w-type zeolite that contains exchanges a large amount of excess metal positively charged ion of needs; With the moderate of carrying out initial cationic or highly exchange, these salt itself are expensive, and it is much more expensive than the zeolite of the conventional sorbent material grade of production that this just causes producing these special ion exchange form.For the cost that reduces final form zeolite and prevent that these ions are discharged in the environment; Must carry out very big effort; From residual exchange solution and washings, reclaim excessive interested ion; Because high-cation exchange capacity W type molecular sieve has very big actual utility value as the high-efficiency adsorbent in environmental protection field, so this problem is the obvious interested problem in environmental protection field.
Usually, contain initial cationic C
iThe w-type zeolite molecular sieve of form is difficult to and final positively charged ion C
fPrimary ions exchanging form through routine makes and contains C
fThe w-type zeolite molecular sieve of form.
Summary of the invention
The object of the present invention is to provide a kind of polynary cationic exchange to produce the method for high-cation exchange capacity W type molecular sieve, to overcome the defective that exists in the known technology.
Be the realization above-mentioned purpose, the method for preparing cation exchange capacity w-type zeolite molecular sieve provided by the invention, key step is:
A) will contain initial cationic C
iThe w-type zeolite molecular sieve of form contacts with the water-soluble ammonium compound that contains ammonium ion, (NH in the w-type zeolite molecular sieve that contains ammonium ion that obtains
4)
2O/Al
2O
3>=0.8;
B) the w-type zeolite molecular sieve that contains ammonium ion that steps A is obtained with contain final positively charged ion C
fSolution contact, with at least a said positively charged ion substituted ammonium ion, and remove volatile ammonia, C in the product that makes from reaction zone
fO/Al
2O
3>=0.7, (NH
4)
2O/Al
2O
3≤0.1;
C) product that step B is obtained is with containing C
fSolution washing, drying finally obtains cation exchange capacity w-type zeolite molecular sieve.
The method for preparing cation exchange capacity w-type zeolite molecular sieve provided by the invention can also be reacted with solid-state heating with final positively charged ion after preparing the w-type zeolite molecular sieve that contains ammonium ion, makes volatile ammonia from system evaporation or distillation.
The w-type zeolite molecular sieve drying that contains ammonium ion that specifically steps A is obtained with contain final positively charged ion C
fPowder mixing post-heating, make volatile ammonia evaporation, C in the product that makes
fO/Al
2O
3>=0.7, (NH
4)
2O/Al
2O
3≤0.1, then with containing C
fSolution washing, drying finally obtains cation exchange capacity w-type zeolite molecular sieve.
Described preparation method, wherein, initial cationic C
iWith final positively charged ion C
fSelectivity coefficient Sf
i f≤0.5.
Described preparation method, wherein, the temperature of reaction of steps A is 0-50 ℃, reaction soln pH is less than 7.
Described preparation method, wherein, the pH value of solution of step B >=7 (preferred pH is greater than 10), temperature is 0-100 ℃.
Described preparation method wherein, washes with purge gas between the reaction period of step B.
Described preparation method, wherein, the water-soluble ammonium compound in the steps A comprises: ammonium sulfate, ammonium chloride, an ammonium nitrate, ammonium acetate or mixture.
Described preparation method, wherein, the final positively charged ion of step B is calcium, sodium ion, mg ion or lithium ion (preferably by calcium ion, recommending calcium ion source to be preferably calcium hydroxide).
The method for preparing high-cation exchange capacity W type molecular sieve provided by the invention need not used a large amount of excessive cationic expensive salt, need not use expensive and the strong positively charged ion recovery scheme of motility simultaneously.
Embodiment
The present invention is a kind of method of utilizing the preparation of polynary cationic exchange to have high-cation exchange capacity W type molecular sieve; At first with the ammonium ion exchange in w-type zeolite molecular sieve and the ammonium thing; Replace the positively charged ion in the w-type zeolite molecular sieve with ammonium ion thus; The w-type zeolite that to cross with ammonium ion exchange then with contain final cationic solution and contact; The pH that keeps solution simultaneously is 9-12, and final acquisition contains final cationic w-type zeolite molecular sieve with high-cation exchange capacity, and wherein the target positively charged ion accounts for more than 70% of w-type zeolite positively charged ion total amount.
Technical scheme of the present invention is specific as follows:
1) will contain initial cationic C
iThe w-type zeolite molecular sieve of form contacts with the water-soluble ammonium compound that contains ammonium ion.Contain initial cationic C
iThe w-type zeolite molecular sieve of form and contain reaction between the water-soluble ammonium compound of ammonium ion and be preferably under about 0-50 ℃ and carry out.This reaction is preferably in less than carrying out under 7 the pH.Water-soluble ammonium compound comprises: the mixture of ammonium sulfate, ammonium chloride, an ammonium nitrate, ammonium acetate or these ammonium compounds.Ammonium concentration is 0.5mol/L-2.5mol/L, and the reaction times is controlled at 2-4h, makes final (NH
4)
2O/Al
2O
3>=0.8; Generally speaking, C
iBe potassium ion.Reaction realizes solid-liquid separation through the centrifugal mode with mixed solution after finishing, and the solid that separation is obtained repeats above-mentioned experiment 3 times, promptly carries out ammonium ion exchange 3 times.Again solid is washed 3 times with the water-soluble ammonium compound that contains ammonium ion at last, centrifugal back decanted solution, the solid sample that obtains is the w-type zeolite molecular sieve that contains ammonium ion.
2) the w-type zeolite molecular sieve that contains ammonium ion that step 1 is obtained with contain final positively charged ion C
fSolution contact, with at least a final positively charged ion substituted ammonium ion, and remove reaction product ammonia from reaction zone.C wherein
iAnd C
fSelectivity coefficient Sf
i f≤0.5, final positively charged ion C
fConcentration is 0.5mol/L-2.5mol/L; PH value of solution>=7 more preferably are higher than 10 times at pH and carry out.In 0-100 ℃ of water-bearing media, react, reaction times 10-24h makes final C
fO/Al
2O
3>=0.7, (NH
4)
2O/Al
2O
3≤0.1; This reaction during reaction with the purge gas flushing, is guaranteed to remove volatile reaction product ammonia from reaction zone.Generally speaking, the positively charged ion of substituted ammonium ion is calcium, sodium ion, mg ion or lithium ion.Aspect more preferably, ammonium ion replaces with calcium ion.Aspect more preferably, calcium ion source is preferably calcium hydroxide.
By substituted w-type zeolite molecular sieve of ammonium ion and final positively charged ion C
fReaction also can carry out with solid-state, for example carry out with dryness basically.Aspect this, this reaction is preferably under about 100-400 ℃ to be carried out.Wherein at least a reaction product (as by the substituted w-type zeolite molecular sieve of ammonium ion) is a gaseous state or volatile, from system evaporation or distillation.
3) the W type molecular sieve that step 2 is obtained is with containing C
fConcentration is the solution washing of 0.02mol/L, and drying finally obtains high-cation exchange capacity w-type zeolite molecular sieve.
The present invention's preparation has high-cation exchange capacity W type molecular sieve, has overcome the problem of present implementation method.Compare with other method of producing high-cation exchange capacity W type molecular sieve, present method need not used a large amount of excessive expensive exchange cation salt, need not use expensive positively charged ion recovery scheme simultaneously.Ion exchange method of the present invention is carried out under the condition of removing a kind of reaction product from reaction zone.IX can be carried out in liquid phase, and wherein a kind of reaction product is a gaseous state or volatile, can blow out reaction zone; Perhaps IX can be solid state reaction, wherein also is that at least a reaction product is a gaseous state or volatile, from system evaporation or distillation.
Embodiment 1
1) 30g is contained the w-type zeolite molecular sieve k of potassium ion
2W and 2L concentration are the ammoniumsulphate soln reaction of 2mol/L.PH value of solution is 6.5, is reflected under the room temperature (25 ℃) to carry out, and the reaction times is 2h, realizes solid-liquid separation through the centrifugal mode then.The solid that separation is obtained repeats above-mentioned experiment 3 times, promptly carries out ammonium ion exchange 3 times.Use 2L concentration to be the ammoniumsulphate soln of 0.01mol/L washing 3 times solid at last, 1. centrifugal back decanted solution obtains sample, and 1. sample is carried out proximate analysis.
2) sample that 10g step 1 is obtained 1. (the w-type zeolite molecular sieve that contains ammonium ion) is the Ca (OH) of 2mol/L with 1L concentration
2Solution reaction is blown into nitrogen to prevent CO in solution in the reaction process
2Get in the solution and Ca (OH)
2React, and remove reaction product ammonia from reaction zone.60 ℃ of temperature of reaction, reaction times 18h, and pH of mixed remains at 9-12 in the 18h of reaction.After reaction is accomplished, with acid pH of mixed is transferred to about 7.0, then that mixed solution is centrifugal, decanted solution obtains solid sample again.
3) solid sample that step 2 is obtained uses the Ca (OH) of 1L concentration as 0.02mol/L
2Solution washing, centrifugal, it is dry again to obtain solid behind the decanted solution, finally obtains the w-type zeolite molecular sieve 2., and 2. sample is carried out proximate analysis.
4) the 2. also residual lower ammonium ion of w-type zeolite molecular sieve that obtains of step 3 adopts 500ml to contain 2mol/L CaCl
2/ NaCl (CaCl
2Be 1.5mol/L, NaCl is 0.5mol/L) 2. react with the w-type zeolite molecular sieve, 60 ℃ of temperature of reaction, reaction times 24h, and pH of mixed remains at 9-12 in the 24h of reaction.After reaction is accomplished, with acid pH of mixed is transferred to about 7.0, then that mixed solution is centrifugal, decanted solution obtains solid sample again.
(5) solid sample that step (4) is obtained uses the CaCl of 500ml concentration as 0.02mol/L
2Solution washing 33 times, centrifugal, it is dry again to obtain solid behind the decanted solution, finally obtains the w-type zeolite molecular sieve 3., and 3. sample is carried out proximate analysis.The chemical composition analysis result that 3. 1., 2. W type molecular sieve reach sees table 1.
Table 1:W type molecular sieve chemical composition analysis
Embodiment 2:
1) will contain initial cationic C
iThe w-type zeolite molecular sieve of form contacts with the water-soluble ammonium compound that contains ammonium ion.Contain initial cationic C
iThe w-type zeolite molecular sieve of form and contain reaction between the water-soluble ammonium compound of ammonium ion and be preferably under about 0-50 ℃ and carry out.This reaction is preferably in less than carrying out under 7 the pH.Water-soluble ammonium compound comprises: the mixture of ammonium sulfate, ammonium chloride, an ammonium nitrate, ammonium acetate or these ammonium compounds.Ammonium concentration is 0.005mol/L-0.1mol/L, and the reaction times is controlled at 2-4h, makes final (NH
4)
2O/Al
2O
3>=0.8; Generally speaking, C
iBe potassium ion.
2) by substituted w-type zeolite molecular sieve of ammonium ion and final positively charged ion C
fReaction also can carry out with solid-state, for example carry out with dryness basically.This reaction is preferably under about 100-400 ℃ to be carried out.Wherein at least a reaction product is a gaseous state or volatile, from system evaporation or distillation.
3) the W type molecular sieve that step 2 is obtained is with containing final positively charged ion C
fConcentration is the solution washing of 0.002mol/L, and drying finally obtains high-cation exchange capacity w-type zeolite molecular sieve.
Claims (8)
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|---|---|---|---|
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| Publication Number | Publication Date |
|---|---|
| CN102491362A true CN102491362A (en) | 2012-06-13 |
Family
ID=46183233
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1196976A (en) * | 1996-12-27 | 1998-10-28 | 美国Boc氧气集团有限公司 | Method of manufacture of molecular sieves |
-
2011
- 2011-11-28 CN CN2011103837103A patent/CN102491362A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1196976A (en) * | 1996-12-27 | 1998-10-28 | 美国Boc氧气集团有限公司 | Method of manufacture of molecular sieves |
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Application publication date: 20120613 |