CN104445258A - LSX powder synthesized by using solid powder guiding agent and preparation method thereof - Google Patents

LSX powder synthesized by using solid powder guiding agent and preparation method thereof Download PDF

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Publication number
CN104445258A
CN104445258A CN201410651105.3A CN201410651105A CN104445258A CN 104445258 A CN104445258 A CN 104445258A CN 201410651105 A CN201410651105 A CN 201410651105A CN 104445258 A CN104445258 A CN 104445258A
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solution
powder
sio
solid
water
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王洪亮
胡宏杰
金梅
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Zhengzhou Fulong New Material Technology Co ltd
Zhengzhou Institute of Multipurpose Utilization of Mineral Resources CAGS
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Zhengzhou Fulong New Material Technology Co ltd
Zhengzhou Institute of Multipurpose Utilization of Mineral Resources CAGS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/20—Faujasite type, e.g. type X or Y
    • C01B39/22—Type X

Abstract

The invention discloses LSX powder synthesized by using a solid powder guiding agent, which comprises the following components in molar ratio: n 2O)/n(Na2O+K2O)=15～25，n(Na2O)/n(Na2O+K2O)=0.70～0.85，n(SiO2)/n(Al2O3)=1.8～2.3，n(Na2O+K2O)/n(SiO2)= 3.00-4.00; the solid powder guiding agent comprises the following components in molar ratio: n 2O)/n(Na2O+K2O)=15～25，n(Na2O)/n(Na2O+K2O)=0.70～0.85，n(SiO2)/n(Al2O3)=1.8～2.3，n(Na2O+K2O)/n(SiO2)And (3) 3.00-4.00. Compared with the prior art, the invention has the beneficial effects that: after the solid powder guiding agent is added, the production period of powder preparation is shortened, and the production cost is relatively reduced; the added solid powder guiding agent has better activity, and the activity retention time is long after drying, thereby avoiding the defects that the liquid guiding agent is repeatedly prepared and the activity is easy to inactivate; synthetic LSX (SiO)2/Al2O3About 2.0) high purity, excellent adsorption performance and good stability.

Description

A kind of LSX powder utilizing solid powder directed agents to synthesize and preparation method thereof
Technical field
The invention belongs to inorganic materials-molecular sieve powder preparing technical field, be specifically related to a kind of LSX powder utilizing solid powder directed agents to synthesize and preparation method thereof.
Background technology
LSX(SiO 2/ Al 2o 3≈ 2.0) former powder is a kind of n (SiO 2)/n (Al 2o 3) be about 2.0 X-type molecular sieve powder, when utilizing its preparative body LSX molecular sieve, generally accounting for 75 ~ 90% of total mass, is most important absorption feed composition.
Its synthetic method of lot of domestic and international bibliographical information, LSX(SiO 2/ Al 2o 3≈ 2.0) raw material sources of former powder are harsh, formula synthesis narrow range, production cycle are long, these factors constrain the powder scale operation that absorption property is high, quality stability is good, cause its production cost higher, compared with external LSX molecular sieve performance, also there is a certain distance.At present, LSX(SiO is synthesized 2/ Al 2o 3≈ 2.0) former powder mainly contains two kinds of modes: one does not add directing agent method to synthesize former powder, and this method production cycle is relatively long, is not easy to suitability for industrialized production; Another kind is that directing agent method synthesizes former powder with solidliquid mixture, and the preparation of this method directed agents is loaded down with trivial details.
Summary of the invention
The technical problem to be solved in the present invention how to adopt simple and effective way to obtain LSX(SiO with short production cycle, production technique is simple, absorption property is high, quality stability is good 2/ Al 2o 3≈ 2.0) former powder, for solving the problem, the invention provides a kind of LSX powder utilizing solid powder directed agents to synthesize and preparation method thereof.
The object of the invention is to realize in the following manner:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=15 ~ 25, n (Na 2o)/n (Na 2o+K 2o)=0.70 ~ 0.85, n (SiO 2)/n (Al 2o 3)=1.8 ~ 2.3, n (Na 2o+K 2o)/n (SiO 2)=3.00 ~ 4.00.
The mol ratio of each component of described solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=15 ~ 25, n (Na 2o)/n (Na 2o+K 2o)=0.70 ~ 0.85, n (SiO 2)/n (Al 2o 3)=1.8 ~ 2.3, n (Na 2o+K 2o)/n (SiO 2)=3.00 ~ 4.00.
The concrete operation step of described LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.05 ~ 2% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40 ~ 60min, by the gel aging 12 ~ 24h at 45 ~ 65 DEG C generated, then crystallization 1 ~ 4h at 90 ~ 100 DEG C;
(5) after reaction terminates, by product suction filtration, be washed with water to PH=9 ~ 10, at 80 ~ 150 DEG C, dry 2 ~ 5h.
The concrete operation step of the preparation of described solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40 ~ 60min, by the gel aging 24 ~ 48h at 40 ~ 50 DEG C generated;
(5) at room temperature airtight placement 12 ~ 48h, then washs to PH=9 ~ 10, dries.
Relative to prior art, beneficial effect of the present invention is:
(1), after adding solid powder directed agents, the production cycle prepared by powder shortens, and relatively reduces production cost.
(2) the solid powder directed agents added is better active, and after drying, activity-maintaining time is long, avoids liquid directed agents and repeatedly prepares and the shortcoming of active easily inactivation.
(3) LSX(SiO synthesized 2/ Al 2o 3≈ 2.0) purity of former powder is high, absorption property is excellent and good stability.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the former powder of LSX that embodiment 8 obtains.
Fig. 2 is the SEM figure of the former powder of LSX that embodiment 8 obtains.
Embodiment
Raw material used in embodiment, silicon raw material is mainly the silicon-dioxide, silica flour, silicon sol etc. of technical grade; Aluminum feedstock is mainly the aluminium hydroxide, aluminum oxide, sodium metaaluminate etc. of technical grade; Sodium potassium highly basic raw material is mainly flaky sodium hydrate and the hydroxide flake potassium of technical grade.According to GB/T6287-1986, at 25 DEG C, under 75%RH condition, detect the saturated static H of former powder 2o adsorptive value.According to GB/T10505.3-1989, detect the static CO of former powder 2adsorptive value.Utilize atomic absorption method to chemically examine the sial content of powder, calculate powder silica alumina ratio n (SiO 2)/n (Al 2o 3).
Embodiment 1:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=15 ~ 25, n (Na 2o)/n (Na 2o+K 2o)=0.70 ~ 0.85, n (SiO 2)/n (Al 2o 3)=1.8 ~ 2.3, n (Na 2o+K 2o)/n (SiO 2)=3.00 ~ 4.00.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=15 ~ 25, n (Na 2o)/n (Na 2o+K 2o)=0.70 ~ 0.85, n (SiO 2)/n (Al 2o 3)=1.8 ~ 2.3, n (Na 2o+K 2o)/n (SiO 2)=3.00 ~ 4.00.
The concrete operation step of described LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.05 ~ 2% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40 ~ 60min, by the gel aging 12 ~ 24h at 45 ~ 65 DEG C generated, then crystallization 1 ~ 4h at 90 ~ 100 DEG C;
(5) after reaction terminates, by product suction filtration, be washed with water to PH=9 ~ 10, at 80 ~ 150 DEG C, dry 2 ~ 5h.
The concrete operation step of the preparation of described solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40 ~ 60min, by the gel aging 24 ~ 48h at 40 ~ 50 DEG C generated;
(5) at room temperature airtight placement 12 ~ 48h, then washs to PH=9 ~ 10, dries.
Embodiment 2:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=15, n (Na 2o)/n (Na 2o+K 2o)=0.70, n (SiO 2)/n (Al 2o 3)=1.8, n (Na 2o+K 2o)/n (SiO 2)=3.00.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=15, n (Na 2o)/n (Na 2o+K 2o)=0.70, n (SiO 2)/n (Al 2o 3)=1.8, n (Na 2o+K 2o)/n (SiO 2)=3.00.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40min, by the gel aging 24h at 40 DEG C generated;
(5) at room temperature airtight placement 12h, then washs to PH=9, dries.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.05% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40min, by the gel aging 12h at 45 DEG C generated, then crystallization 1h at 90 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9, at 80 DEG C, dry 2h.
Embodiment 3:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=17, n (Na 2o)/n (Na 2o+K 2o)=0.73, n (SiO 2)/n (Al 2o 3)=1.9, n (Na 2o+K 2o)/n (SiO 2)=3.20.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=17, n (Na 2o)/n (Na 2o+K 2o)=0.73, n (SiO 2)/n (Al 2o 3)=1.9, n (Na 2o+K 2o)/n (SiO 2)=3.20.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 44min, by the gel aging 29h at 42 DEG C generated;
(5) at room temperature airtight placement 20h, then washs to PH=9.2, dries.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.50% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 44min, by the gel aging 15h at 49 DEG C generated, then crystallization 1.5h at 92 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9.2, at 90 DEG C, dry 3h.
Embodiment 4:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=19, n (Na 2o)/n (Na 2o+K 2o)=0.76, n (SiO 2)/n (Al 2o 3)=2.0, n (Na 2o+K 2o)/n (SiO 2)=3.40.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=19, n (Na 2o)/n (Na 2o+K 2o)=0.76, n (SiO 2)/n (Al 2o 3)=2.0, n (Na 2o+K 2o)/n (SiO 2)=3.40.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 48min, by the gel aging 34h at 44 DEG C generated;
(5) at room temperature airtight placement 28h, then washs to PH=9.4, dries.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.90% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 48min, by the gel aging 18h at 53 DEG C generated, then crystallization 2h at 94 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9.4, at 100 DEG C, dry 4h.
Embodiment 5:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=21, n (Na 2o)/n (Na 2o+K 2o)=0.79, n (SiO 2)/n (Al 2o 3)=2.1, n (Na 2o+K 2o)/n (SiO 2)=3.60.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=21, n (Na 2o)/n (Na 2o+K 2o)=0.79, n (SiO 2)/n (Al 2o 3)=2.1, n (Na 2o+K 2o)/n (SiO 2)=3.60.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 52min, by the gel aging 39h at 46 DEG C generated;
(5) at room temperature airtight placement 36h, then washs to PH=9.6, dries.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 1.20% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 52min, by the gel aging 21h at 57 DEG C generated, then crystallization 2.5h at 96 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9.6, at 110 DEG C, dry 2.5h.
Embodiment 6:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=23, n (Na 2o)/n (Na 2o+K 2o)=0.82, n (SiO 2)/n (Al 2o 3)=2.2, n (Na 2o+K 2o)/n (SiO 2)=3.80.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=23, n (Na 2o)/n (Na 2o+K 2o)=0.82, n (SiO 2)/n (Al 2o 3)=2.2, n (Na 2o+K 2o)/n (SiO 2)=3.80.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 56min, by the gel aging 44h at 48 DEG C generated;
(5) at room temperature airtight placement 42h, then washs to PH=9.8, dries.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 1.60% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 56min, by the gel aging 22h at 61 DEG C generated, then crystallization 3h at 98 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9.8, at 120 DEG C, dry 5h.
Embodiment 7:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=25, n (Na 2o)/n (Na 2o+K 2o)=0.85, n (SiO 2)/n (Al 2o 3)=2.3, n (Na 2o+K 2o)/n (SiO 2)=4.00.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=25, n (Na 2o)/n (Na 2o+K 2o)=0.85, n (SiO 2)/n (Al 2o 3)=2.3, n (Na 2o+K 2o)/n (SiO 2)=4.00.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 60min, by the gel aging 48h at 50 DEG C generated;
(5) at room temperature airtight placement 48h, then washs to PH=10, dries.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 2.0% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 60min, by the gel aging 24h at 65 DEG C generated, then crystallization 4h at 100 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=10, at 130 DEG C, dry 4.5h.
Embodiment 8:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=17, n (Na 2o)/n (Na 2o+K 2o)=0.77, n (SiO 2)/n (Al 2o 3)=2.0, n (Na 2o+K 2o)/n (SiO 2)=3.25.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=17, n (Na 2o)/n (Na 2o+K 2o)=0.75, n (SiO 2)/n (Al 2o 3)=2.0, n (Na 2o+K 2o)/n (SiO 2)=3.25.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 50min, by the gel aging 30h at 40 DEG C generated;
(5) at room temperature airtight placement 18h, then washs to PH=9, dries, obtains solid powder directed agents.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.10% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 50min, by the gel aging 20h at 50 DEG C generated, then crystallization 2h at 100 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9, at 140 DEG C, dry 2h.
After tested, the saturated static H2O adsorptive value of former powder is 32.10%, static CO 2adsorptive value is 21.68%, the n (SiO of powder 2)/n (Al 2o 3)=2.01, its XRD figure and SEM figure are shown in Fig. 1 and Fig. 2 respectively.
The contrast experiment of embodiment 8:
Except not reinforcing body powder directed agents, all the other experiment conditions are with identical in embodiment 8, and experiment records the saturated static H of former powder 2o adsorptive value is 29.03%, static CO 2adsorptive value is 19.34%.
Contrasted by embodiment 8 can obtain with its contrast experiment, not reinforcing body powder directed agents, LSX(SiO 2/ Al 2o 3≈ 2.0) H of former powder 2o adsorptive value obviously reduces.
Embodiment 9:
Utilize the LSX powder that solid powder directed agents is synthesized, the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=22, n (Na 2o)/n (Na 2o+K 2o)=0.77, n (SiO 2)/n (Al 2o 3)=2.04, n (Na 2o+K 2o)/n (SiO 2)=3.75.
The mol ratio of each component of solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=18, n (Na 2o)/n (Na 2o+K 2o)=0.75, n (SiO 2)/n (Al 2o 3)=2.0, n (Na 2o+K 2o)/n (SiO 2)=3.30.
The concrete operation step of the preparation of solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 45min, by the gel aging 20h at 50 DEG C generated;
(5) at room temperature airtight placement 16h, then washs to PH=9.2, dries, obtains solid powder directed agents.
The concrete operation step of LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.20% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 45min, by the gel aging 18h at 55 DEG C generated, then crystallization 3h at 95 DEG C;
(5), after reaction terminates, by product suction filtration, be washed with water to PH=9.2, at 150 DEG C, dry 2h.
After tested, the saturated static H2O adsorptive value of former powder is 32.45%, static CO 2adsorptive value is 22.67%, the n (SiO of powder 2)/n (Al 2o 3)=2.00.
The contrast experiment of embodiment 9:
Except not reinforcing body powder directed agents, all the other experiment conditions are with identical in embodiment 9, and experiment records the saturated static H of former powder 2o adsorptive value is 28.46%, static CO 2adsorptive value is 19.20%.
Contrasted by embodiment 9 can obtain with its contrast experiment, not reinforcing body powder directed agents, LSX(SiO 2/ Al 2o 3≈ 2.0) H of former powder 2o adsorptive value obviously reduces.

Claims (4)

1. utilize the LSX powder that solid powder directed agents is synthesized, it is characterized in that: the mol ratio of each component is: n (H 2o)/n (Na 2o+K 2o)=15 ~ 25, n (Na 2o)/n (Na 2o+K 2o)=0.70 ~ 0.85, n (SiO 2)/n (Al 2o 3)=1.8 ~ 2.3, n (Na 2o+K 2o)/n (SiO 2)=3.00 ~ 4.00.
2. a kind of LSX powder utilizing solid powder directed agents to synthesize according to claim 1, is characterized in that: the mol ratio of each component of described solid powder directed agents is: n (H 2o)/n (Na 2o+K 2o)=15 ~ 25, n (Na 2o)/n (Na 2o+K 2o)=0.70 ~ 0.85, n (SiO 2)/n (Al 2o 3)=1.8 ~ 2.3, n (Na 2o+K 2o)/n (SiO 2)=3.00 ~ 4.00.
3. a kind of LSX raw powder's production technology utilizing solid powder directed agents to synthesize according to claim 1, is characterized in that: the concrete operation step of described LSX powder is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, add solid powder directed agents (accounting for 0.05 ~ 2% of mixture total mass), mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40 ~ 60min, by the gel aging 12 ~ 24h at 45 ~ 65 DEG C generated, then crystallization 1 ~ 4h at 90 ~ 100 DEG C;
(5) after reaction terminates, by product suction filtration, be washed with water to PH=9 ~ 10, at 80 ~ 150 DEG C, dry 2 ~ 5h.
4. a kind of LSX raw powder's production technology utilizing solid powder directed agents to synthesize according to claim 3, is characterized in that: the concrete operation step of the preparation of described solid powder directed agents is:
(1) sample according to mol ratio;
(2) solid NaOH is dissolved in water is mixed with NaOH solution, boil, add powdery Al (OH) 3, until solution becomes clear, be mixed with NaAlO 2solution;
(3) KOH solution will prepared with solid KOH, adds the NaAlO prepared 2in solution, mixing and stirring;
(4) water glass solution prepared according to certain liquid glass and water is under agitation added, mix and blend 40 ~ 60min, by the gel aging 24 ~ 48h at 40 ~ 50 DEG C generated;
(5) at room temperature airtight placement 12 ~ 48h, then washs to PH=9 ~ 10, dries.
CN201410651105.3A 2014-11-17 2014-11-17 LSX powder synthesized by using solid powder guiding agent and preparation method thereof Pending CN104445258A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1178771A (en) * 1996-07-12 1998-04-15 策卡有限公司 Synthetic LSX faujasite by reactor using Archimedian screw rod stirrer
CN101289197A (en) * 2008-06-13 2008-10-22 洛阳市建龙化工有限公司 Method for preparing low-silicon X-shaped molecular screen LSX
CN102874837A (en) * 2011-07-11 2013-01-16 中国石油化工股份有限公司 Preparation method of low silica aluminium molecular sieve LSX directly synthesized from kaolin
CN103214002A (en) * 2013-04-09 2013-07-24 洛阳市建龙化工有限公司 Method for preparing small crystal grain X type molecular sieve raw powder
CN103387241A (en) * 2012-05-11 2013-11-13 华东理工大学 Amine-free rapid in-situ crystallization ZSM-5 molecular sieve synthesis method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1178771A (en) * 1996-07-12 1998-04-15 策卡有限公司 Synthetic LSX faujasite by reactor using Archimedian screw rod stirrer
CN101289197A (en) * 2008-06-13 2008-10-22 洛阳市建龙化工有限公司 Method for preparing low-silicon X-shaped molecular screen LSX
CN102874837A (en) * 2011-07-11 2013-01-16 中国石油化工股份有限公司 Preparation method of low silica aluminium molecular sieve LSX directly synthesized from kaolin
CN103387241A (en) * 2012-05-11 2013-11-13 华东理工大学 Amine-free rapid in-situ crystallization ZSM-5 molecular sieve synthesis method
CN103214002A (en) * 2013-04-09 2013-07-24 洛阳市建龙化工有限公司 Method for preparing small crystal grain X type molecular sieve raw powder

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