CN101717094A - Sodium-type low-silicon X-type molecular sieve raw powder and preparation method thereof - Google Patents
Sodium-type low-silicon X-type molecular sieve raw powder and preparation method thereof Download PDFInfo
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- CN101717094A CN101717094A CN200910227251A CN200910227251A CN101717094A CN 101717094 A CN101717094 A CN 101717094A CN 200910227251 A CN200910227251 A CN 200910227251A CN 200910227251 A CN200910227251 A CN 200910227251A CN 101717094 A CN101717094 A CN 101717094A
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- molecular sieve
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Abstract
The invention discloses a sodium-type low-silicon X-type molecular sieve raw powder (NaLSX for short) and a preparation method thereof. The molar ratio of all components of NaLSX are as follows: K2O/Al2O3=0-0.05, Na2O/Al2O3= 0.95-1.00, SiO2/Al2O3=2.0-2.1 and (K2O+Na2O)/Al2O3=1.00; the method comprises the following steps of: firstly preparing a sodium-type low-silicon X-type molecular sieve of SiO2/Al2O3=2.0-2.1; then using a sodium salt solution of 0.5-1.5M to carry out Na+ exchange for 1-2 hours at the temperature of 70-75 DEG C, washing and drying, and then preparing the NaLSX molecular sieve. The molecular sieve raw powder has high Na+ exchange degree, high molecular sieve crystallinity, high adsorption capacity, high adsorption rate and low cost, and has higher capability of removing H2O and CO2 in air; the raw powder is more superior if serving as the raw material for preparing LiLSX molecular sieve O2 separation adsorbents.
Description
Technical field
The present invention relates to a kind of sieve technology, relate to a kind of sodium-type low-silicon X-type molecular sieve raw powder and preparation method thereof specifically.
Technical background
Low-silicon X-shaped molecular screen is called for short LSX, works as SiO
2/ Al
2O
3Mol ratio is 2.0-2.1, and its cation-bit reaches maximum value, has maximum adsorption centers.Common sodium-type low-silicon X-type molecular sieve is called for short NaLSX.Molecular sieve is the synthetic low-silicon X-shaped molecular screen in the K-Na mixed system, contains Na
+And K
+Two kinds of positively charged ions also can be called for short KNaLSX, wherein K
+Account for 25%, Na
+Account for 75%.At present, the existing lot of documents report of the preparation method of KNaLSX molecular sieve, but synthesis type low-silicon X-shaped molecular screen KNaLSX is also not obvious to the superiority of the absorption of water and carbonic acid gas.From positively charged ion absorption property is influenced consideration, sodium-type low-silicon X-type molecular sieve, the performance more superior to being adsorbed with of water and carbonic acid gas.But with the sodium type X type molecular sieve of synthetic method preparation, its SiO
2/ Al
2O
3Mol ratio is at 2.35-2.55, and directly the synthetic method can not prepare SiO
2/ Al
2O
3Mol ratio is the sodium-type low-silicon X-type molecular sieve NaLSX of (2.0-2.1).
The technical current demand that the raising low-silicon X-shaped molecular screen is arranged the loading capacity of water and carbonic acid gas.But, also directly not synthetic at present SiO
2/ Al
2O
3Mol ratio is the technology of the higher low-silicon X-shaped molecular screen of the loading capacity to water and carbonic acid gas of 2.0-2.1.
Summary of the invention
One of technical problem to be solved of the present invention is to provide a kind of sodium-type low-silicon X-type molecular sieve raw powder, can have than high-adsorption-capacity and adsorption rate water and carbonic acid gas.
The technical problem that the present invention further solves provides a kind of preparation method of above-mentioned molecular screen primary powder.
In order to reach the purpose that solves the problems of the technologies described above, a kind of sodium-type low-silicon X-type molecular sieve raw powder of the present invention, the mol ratio of each component is: K
2O/Al
2O
3=0-0.05; Na
2O/Al
2O
3=0.95-1.00; SiO
2/ Al
2O
3=2.0-2.1, wherein (K
2O+Na
2O)/Al
2O
3=1.00.
Described a kind of sodium-type low-silicon X-type molecular sieve raw powder, its further the mol ratio of preferred each component can be K
2O/Al
2O
3=0-0.02; Na
2O/Al
2O
3=0.98-1.00.
Described a kind of sodium-type low-silicon X-type molecular sieve raw powder, its further the mol ratio of preferred each component can also be SiO
2/ Al
2O
3=2.0.
A kind of sodium-type low-silicon X-type molecular sieve raw powder, preparation method thereof of the present invention, its step is as follows:
1, according to preparation mol ratio SiO
2/ Al
2O
3The potassium sodium-type low-silicon X-type molecular sieve KNaLSX prior art of=2.0-2.1, preparation SiO
2/ Al
2O
3The potassium sodium-type low-silicon X-type molecular sieve KNaLSX of=2.0-2.1.The method that concrete technology of preparing scheme can provide for " Crystallization of low-silica Faujasite " paper in Zeoliters (1987) 7 phase the 451st page head according to Gunter H.Kuhl.
2, use NaCl, the NaNO of 0.5-1.5M
3And Na
2SO
4A kind of solution in the solution or its mixing solutions and KNaLSX molecular sieve carry out Na
+Exchange is pressed NaCl and is calculated, butt KNaLSX/ butt NaCl mass ratio=(1.5-2.3)/1, Na
+The exchange temperature is 70-75 ℃, time 1-2 hour, filter, and repeat 2-3 time, be washed till no Cl
-, the NaLSX molecular sieve is made in oven dry.
A kind of sodium-type low-silicon X-type molecular sieve raw powder, preparation method thereof of the present invention, further concrete technical scheme can be: described NaCl, NaNO
3And Na
2SO
4The used Na that contains in a kind of solution in the solution or its mixing solutions
+The CaO/MgO mass content is less than 0.02% in the salt, and PH is 6.5-8.5.
A kind of sodium-type low-silicon X-type molecular sieve raw powder, preparation method thereof of the present invention, further concrete technical scheme can also be: described NaCl, NaNO
3And Na
2SO
4Used deionized water and washing process deionized water in a kind of solution in the solution or its mixing solutions, its CaO/MgO content calculate by CaO and are lower than 5mg/l.
A kind of sodium-type low-silicon X-type molecular sieve raw powder, preparation method thereof of the present invention, further concrete technical scheme can also be: described NaCl, NaNO
3And Na
2SO
4A kind of solution in the solution or its mixing solutions with KNaLSX molecular sieve exchange process in repeatedly recycle, the method that recycles is for containing Na through exchange
+Measure low NaCl, NaNO
3And Na
2SO
4A kind of solution in the solution or its mixing solutions with contain K
+Measure the contact earlier of high molecular sieve, contain K through metathetical then
+Measure low molecular sieve again with contain Na
+Measure high NaCl, NaNO
3And Na
2SO
4A kind of solution or its mixing solutions in the solution further exchange.
NaLSX molecular screen primary powder of the present invention, its application comprise the sorbent material that is used for preparing oxygen technology and as the raw material of preparation LiLSX molecular sieve making oxygen by air separation sorbent material.The consumption maximum be the sorbent material that is used for preparing oxygen technology, raw air is purified, remove H wherein
2O and CO
2, its adsorptive capacity and adsorption rate compare SiO
2/ Al
2O
3The common X molecular sieve and the KNaLSX molecular screen primary powder of=2.35-2.55 molar ratio are more superior; When conduct prepares the raw material of LiLSX molecular sieve making oxygen by air separation sorbent material, at Li
+Make raw material ratio with NaLSX in the exchange process and make raw material with KNaLSX, the process that reclaims Li in the filtrate is easier, can improve the utilization ratio of Li, reduces the LiLSX manufacturing cost.
The KNaLSX molecular sieve of preparation in its step 1, at 25 ℃, P/P
0Under=0.21 the situation, the hexanaphthene saturated extent of adsorption is 17.0%, and at 25 ℃, under the situation of relative humidity 50%, water regain is 30.0%, at 25 ℃, and under the situation of pressure 250mmHg, CO
2Adsorptive capacity is 20.0%.
Sodium-type low-silicon X-type provided by the invention (NaLSX) molecular sieve than synthesis type KNaLSX molecular sieve to water and CO
2Loading capacity improve 6-8% and 10-15% respectively.
By adopting above-mentioned technical scheme, the former powder of the NaLSX that a kind of sodium-type low-silicon X-type molecular sieve raw powder of the present invention and preparation method thereof provides, its Na
+Exchange degree height, molecular sieve crystallinity height, loading capacity is big, adsorption rate is fast, cost is low, has better to remove H in the air
2O and CO
2Ability; Raw material as preparation LiLSX molecular sieve making oxygen by air separation sorbent material is more superior.
Embodiment
Below by example technology of the present invention is awarded further instruction, but the claimed content of the present invention is not limited to these examples.
Raw material used in following examples is:
KNaLSX (low-silicon X-shaped) molecular sieve: by the method that Gunter H.Kuhl provides for " Crystallization of low-silica Faujasite " paper in Zeoliters (1987) 7 phase the 451st page head, preparation mol ratio SiO
2/ Al
2O
3=2.0 potassium sodium-type low-silicon X-type molecular sieve KNaLSX, during its mol ratio is formed, SiO
2/ Al
2O
3=2.0, K
2O/ (K
2O+Na
2O)=and 0.20-0.25, (K
2O+Na
2O)/Al
2O
3=1.00.At 25 ℃, P/P
0Under=0.21 the situation, the hexanaphthene saturated extent of adsorption is 17.0%; At 25 ℃, under the situation of relative humidity 50%, water regain is 30.0%; At 25 ℃, under the situation of pressure 250mmHg, CO
2Adsorptive capacity is 20.0%.
Contain Na salt and select refining NaCl for use, the NaCl mass content is greater than 99.5%, and the CaO/MgO mass content is less than 0.02%.
Deionized water: CaO/MgO content is less than 5mg/l.
Embodiment 1:
The NaCl solution that with 600ml concentration is 1.1M earlier adds in the exchange still, under agitation the former powder of 38 gram KNaLSX is slowly added in the still, is warming up to 70 ℃ gradually, and constant temperature 45 minutes filters, and uses the 600ml deionized water wash, and the triplicate exchange is washed till no Cl for the last time
-, dry under 110 ℃, promptly get the NaLSX product, record Na
+Exchange degree is 98.60%, and water regain is 31.77%, CO
2Adsorptive capacity is 22.51%.
Embodiment 2:
60 liters of NaCl solution with 1.1M add in the exchange still earlier, under agitation the former powder of 3.8kg KNaLSX are slowly added in the still, are warming up to 75 ℃ gradually, and constant temperature 1 hour filters, and with 60 liters of deionized water wash, the triplicate exchange is washed till no Cl for the last time
-, dry under 110 ℃, promptly get the NaLSX product, record Na
+Exchange degree is 98.48%, and water regain is 31.80%, CO
2Adsorptive capacity is 22.56%.
Embodiment 3:
As the operation of embodiment 2, be the Na first time
+The filtrate that exchanges for the third time in the exchange use-case 2, twice Na in back
+Exchange with fresh NaCl solution, product Na
+Exchange degree is 98.45%, and water regain is 31.80%, CO
2Adsorptive capacity is 22.50%.
Claims (7)
1. sodium-type low-silicon X-type molecular sieve raw powder, it is characterized in that: the mol ratio of each component is: K
2O/Al
2O
3=0-0.05, Na
2O/Al
2O
3=0.95-1.00, SiO
2/ Al
2O
3=2.0-2.1, (K
2O+Na
2O)/Al
2O
3=1.00.
2. a kind of according to claim 1 sodium-type low-silicon X-type molecular sieve raw powder, it is characterized in that: the mol ratio of described each component is: K
2O/Al
2O
3=0-0.02; Na
2O/Al
2O
3=0.98-1.00.
3. a kind of according to claim 1 sodium-type low-silicon X-type molecular sieve raw powder, it is characterized in that: the mol ratio of described each component is: SiO
2/ Al
2O
3=2.0.
4. the preparation method of the described sodium-type low-silicon X-type molecular sieve raw powder of claim 1 is characterized in that step is as follows:
---preparation mol ratio SiO
2/ Al
2O
3The potassium sodium-type low-silicon X-type molecular sieve KNaLSX of=2.0-2.1;
---with NaCl, the NaNO of 0.5-1.5M
3And Na
2SO
4A kind of solution in the solution or its mixing solutions and KNaLSX molecular sieve carry out Na
+Exchange is pressed NaCl and is calculated, butt KNaLSX/ butt NaCl mass ratio=(1.5-2.3)/1, Na
+The exchange temperature is 70-75 ℃, time 1-2 hour, filter, and repeat 2-3 time, be washed till no Cl
-, the NaLSX molecular sieve is made in oven dry.
5. as the preparation method of sodium-type low-silicon X-type molecular sieve raw powder as described in the claim 4, it is characterized in that: described NaCl, NaNO
3And Na
2SO
4The used Na that contains in a kind of solution in the solution or its mixing solutions
+The CaO/MgO mass content is less than 0.02% in the salt, and PH is 6.5-8.5.
6. as the preparation method of sodium-type low-silicon X-type molecular sieve raw powder as described in the claim 4, it is characterized in that: described NaCl, NaNO
3And Na
2SO
4Na in a kind of solution in the solution or its mixing solutions
+Exchange liquid and washing deionized water, wherein CaO/MgO content calculates by CaO and is lower than 5mg/l.
7. as the preparation method of sodium-type low-silicon X-type molecular sieve raw powder as described in the claim 4, it is characterized in that: described NaCl, NaNO
3And Na
2SO
4A kind of solution in the solution or its mixing solutions with KNaLSX molecular sieve exchange process in repeatedly recycle, the method that recycles is for containing Na through exchange
+Measure low NaCl, NaNO
3And Na
2SO
4A kind of solution in the solution or its mixing solutions with contain K
+Measure the contact earlier of high molecular sieve, contain K through metathetical then
+Measure low molecular sieve again with contain Na
+Measure high NaCl, NaNO
3And Na
2SO
4A kind of solution or its mixing solutions in the solution further exchange.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247801A (en) * | 2011-05-26 | 2011-11-23 | 洛阳市建龙化工有限公司 | Application of sodium form low-silicon X-type molecular sieve raw powder to preparation of adsorbent |
| CN103721673A (en) * | 2014-01-06 | 2014-04-16 | 郑州富龙新材料科技有限公司 | Preparation method of K-A molecular sieve |
| CN106276968A (en) * | 2016-07-25 | 2017-01-04 | 洛阳市建龙微纳新材料股份有限公司 | The preparation method of a kind of modified HEU type zeolite and the application as nitrogen selected adsorbent |
-
2009
- 2009-11-23 CN CN200910227251A patent/CN101717094A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247801A (en) * | 2011-05-26 | 2011-11-23 | 洛阳市建龙化工有限公司 | Application of sodium form low-silicon X-type molecular sieve raw powder to preparation of adsorbent |
| CN103721673A (en) * | 2014-01-06 | 2014-04-16 | 郑州富龙新材料科技有限公司 | Preparation method of K-A molecular sieve |
| CN106276968A (en) * | 2016-07-25 | 2017-01-04 | 洛阳市建龙微纳新材料股份有限公司 | The preparation method of a kind of modified HEU type zeolite and the application as nitrogen selected adsorbent |
| CN106276968B (en) * | 2016-07-25 | 2018-07-17 | 洛阳建龙微纳新材料股份有限公司 | A kind of preparation method of modified HEU types zeolite and the application as nitrogen selected adsorbent |
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Open date: 20100602 |