CN107551994A - A kind of preparation method of the X-type molecular sieve of adsorbing separation methane nitrogen/LDHs compound adsorbents - Google Patents

A kind of preparation method of the X-type molecular sieve of adsorbing separation methane nitrogen/LDHs compound adsorbents Download PDF

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CN107551994A
CN107551994A CN201711037930.4A CN201711037930A CN107551994A CN 107551994 A CN107551994 A CN 107551994A CN 201711037930 A CN201711037930 A CN 201711037930A CN 107551994 A CN107551994 A CN 107551994A
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molecular sieve
type molecular
ldhs
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王绚
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Yantai Zhiben Intellectual Property Operation and Management Co Ltd
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Yantai Zhiben Intellectual Property Operation and Management Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/047—Pressure swing adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/105—Removal of contaminants of nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/24—Hydrocarbons
    • B01D2256/245—Methane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/102—Nitrogen

Abstract

The present invention relates to a kind of preparation method of the X-type molecular sieve of adsorbing separation methane nitrogen/LDHs compound adsorbents, by the way that X-type molecular sieve and anion surfactant or anionic polyelectrolyte are carried out into reaction modification under hydrothermal condition, so that X-type molecular sieve surface carries negative electrical charge, so as to be combined with each other to form composite with LDHs using the principle of the replaceable insertion of LDHs interlayer anions, the beneficial effects of the invention are as follows：Negatively charged X-type molecular sieve intercalation after anion modified is entered into LDHs interlayers, both the suction-operated of X-type molecular sieve had been make use of, simultaneously because the electrostatic interaction between X-type molecular sieve and LDHs laminates, the distribution of charges of X-type molecular sieve in itself is changed, thus greatly strengthen X-type molecular sieve in PSA techniques to N2Adsorption effect.

Description

A kind of system of the X-type molecular sieve of adsorbing separation methane nitrogen/LDHs compound adsorbents Preparation Method
Technical field
The application is to be directed to Application No. 201610195148.4, and the applying date is on March 31st, 2016, entitled " a kind of Point of the application for a patent for invention of the preparation method of the X-type molecular sieve of pressure swing adsorption/separation of methane nitrogen/LDHs compound adsorbents " Case application.
The present invention relates to a kind of preparation method of adsorbent, more particularly to a kind of compound suction of adsorbing separation methane nitrogen Attached dose of preparation method, belong to adsorbent preparing technical field.
Background technology
Methane is the energy of high effect cleaning and important industrial chemicals, separates and carries from coal bed gas, natural gas, casing-head gas etc. Pure methane, for preserving the ecological environment and alleviating energy crisis all has positive effect.The master of coal bed gas, natural gas casing-head gas etc. It is CO to form2、CH4And N2Deng CO2With CH4The physical property difference of molecule is big, is easily isolated, but N2With CH4Critical-temperature All very low, the two physical property is close, and kinetic diameter is close, is not readily separated, so the key of separation of methane is CH4With nitrogen Efficiently separate.
In recent years, pressure-variable adsorption (pressure swing absorption, PSA) technique is with flexible and convenient operation, investment Less, the good advantage of performance, the technology of greatest concern of concentration methane/nitrogen is become.Influence PSA separation of methane/nitrogen very Crucial factor is adsorbent, and the exploitation to its adsorbent is constantly subjected to global concern, currently used adsorbent one As the more difficult adsorptive selectivity separation requirement for meeting methane/nitrogen.Activated carbon is mostly important widely used adsorbent, still Acticarbon research and development for methane/nitrogen separation are also seldom, and there is presently no the suction of the activated carbon specifically for the system Attached dose of product.
The content of the invention
The present invention is for deficiency existing for adsorbent in methane nitrogen PSA separation, there is provided a kind of pressure swing adsorption/separation of methane The preparation method of the X-type molecular sieve of nitrogen/LDHs compound adsorbents.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation side of the X-type molecular sieve of pressure swing adsorption/separation of methane nitrogen/LDHs compound adsorbents
Method, it is characterised in that comprise the following steps：
1) LDHs preparation：The magnesium salts of solubility and aluminium salt are placed in deionized water dissolving are configured to total concentration and be 0.5mol/L solution A, aqueous slkali B is added dropwise in solution A under constant agitation, keeps pH value of solution in the process Value 9~10, aqueous slkali B continue stirring ageing 3~5 hours, filtering, washed repeatedly to neutrality, by products obtained therefrom after being added dropwise It is placed in 6~10 hours in 80~100 DEG C of baking oven and colloidal sol is made；
2) modification of X-type molecular sieve：By particle diameter 0.1~1 μm of NaX type molecular sieves be added to anionic polyelectrolyte or In the aqueous solution of anion surfactant, ultrasonication 1~3 hour, under the conditions of 50~70 DEG C of stirred in water bath Reaction 4~10 hours, the concentration of aqueous solution of the anionic polyelectrolyte or anion surfactant is 1~10g/L, described NaX types molecular sieve is 1 with the weight ratio of anionic polyelectrolyte or anion surfactant：(0.01~0.1), after having reacted Centrifuge and remove unreacted anionic polyelectrolyte or anion surfactant, obtain the X-type that surface carries negative electrical charge Molecular sieve；
3) preparation of X-type molecular sieve/LDHs compound adsorbents：The X-type molecular sieve of gained in step 2) is added into step 1) In the colloidal sol of gained, the weight ratio of NaX types molecular sieve and colloidal sol is 1：(20~30), after the mixture of the two is placed in 50~70 Ion-exchange reactions is carried out under the conditions of DEG C stirred in water bath, in 6~8 hours reaction time, filtering and washing, is dried after completion of the reaction, Obtain X-type molecular sieve/LDHs compound adsorbents.
Further, aluminium salt described in step 1) and magnesium salts are aluminum nitrate and magnesium nitrate, and the aqueous slkali is that sodium hydroxide is molten Liquid.
Further, the anionic polyelectrolyte described in step 2) is in kayexalate, sodium lignin sulfonate One or more, described anion surfactant are neopelex.
The beneficial effects of the invention are as follows：
1) negatively charged X-type molecular sieve intercalation after anion modified is entered into LDHs interlayers, both make use of X-type molecular sieve Suction-operated, simultaneously because the electrostatic interaction between X-type molecular sieve and LDHs laminates, changes the electric charge of X-type molecular sieve in itself Distribution, thus X-type molecular sieve is greatly strengthen in PSA techniques to N2Adsorption effect；
2) whole preparation process reaction condition is gentle, simple to operate, it is easy to accomplish.
The X-type for pressure swing adsorption/separation of methane/nitrogen point obtained by above-mentioned preparation method is also claimed in the present invention Sub- sieve/LDHs compound adsorbents and its application in pressure swing adsorption/separation of methane/nitrogen.
Embodiment
The principle and feature of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and It is non-to be used to limit the scope of the present invention.
Embodiment 1：
A kind of preparation method of the X-type molecular sieve of pressure swing adsorption/separation of methane nitrogen/LDHs compound adsorbents, including such as Lower step：
1) 150g Al (NO are weighed3)3·9H2O and 51.3g Mg (NO3)2·6H2O is dissolved in 1200mL deionized waters, is matched somebody with somebody It is 0.5molL that total concentration, which is made,-1Mixing salt solution, weigh 80g NaOH and be dissolved in 400ml deionized waters and be configured to 5mol·L-1NaOH solution, NaOH solution is added dropwise in mixing salt solution under agitation, during dropwise addition System pH is kept 9~10, NaOH solution continues stirring ageing 3 hours after being added dropwise, products therefrom is filtered, using going Ionized water is washed 3 times repeatedly, and it is 2wt% hydrotalcite colloidal sol to be placed in 6 hours obtained solid contents in 100 DEG C of thermostatic drying chambers；
2) weigh 0.1~1 μm of NaX type molecular sieves 100g and be added to the kayexalate that 500ml concentration is 6g/L In (abbreviation PSS) aqueous solution, be initially positioned in 20Hz ultrasonic devices ultrasound 2 hours, after be placed in it is anti-under the conditions of 60 DEG C of stirred in water bath Answer 5 hours, centrifuged after having reacted and remove unreacted PSS, obtain the X-type molecular sieve that surface carries negative electrical charge；
3) the X-type molecular sieve 20g of gained in step 2) is taken to be placed in the colloidal sol obtained by 400g steps 1), by the mixing of the two Thing carries out ion-exchange reactions under the conditions of being placed in 50 DEG C of stirred in water bath, filtering and washing after reacting 6 hours, dries, obtains X-type molecule Sieve/LDHs compound adsorbents.
Under conditions of 25 DEG C, 100KPa, the CH of products obtained therefrom4And N2Adsorbance is respectively 16.5cm3/ g and 3.5cm3/ G, the equilibrium separation ratio of methane nitrogen is 4.7.
Embodiment 2：
A kind of preparation method of the X-type molecular sieve of pressure swing adsorption/separation of methane nitrogen/LDHs compound adsorbents, including such as Lower step：
1) 150g Al (NO are weighed3)3·9H2O and 51.3g Mg (NO3)2·6H2O is dissolved in 1200mL deionized waters, is matched somebody with somebody It is 0.5molL that total concentration, which is made,-1Mixing salt solution, weigh 80g NaOH and be dissolved in 400ml deionized waters and be configured to 5mol·L-1NaOH solution, NaOH solution is added dropwise in mixing salt solution under agitation, during dropwise addition System pH is kept 9~10, NaOH solution continues stirring ageing 3 hours after being added dropwise, products therefrom is filtered, using going Ionized water is washed 3 times repeatedly, and it is 2wt% hydrotalcite colloidal sol to be placed in 6 hours obtained solid contents in 100 DEG C of thermostatic drying chambers；
2) weigh 0.1~1 μm of NaX type molecular sieves 100g and be added to the DBSA that 500ml concentration is 1g/L In sodium water solution, be initially positioned in 20Hz ultrasonic devices ultrasound 2 hours, after be placed under the conditions of 70 DEG C of stirred in water bath and react 4 hours, Centrifuged after having reacted and remove unreacted neopelex, obtain the X-type molecular sieve that surface carries negative electrical charge；
3) the X-type molecular sieve 30g of gained in step 2) is taken to be placed in the colloidal sol obtained by 750g steps 1), by the mixing of the two Thing carries out ion-exchange reactions under the conditions of being placed in 60 DEG C of stirred in water bath, filtering and washing after reacting 8 hours, dries, obtains X-type molecule Sieve/LDHs compound adsorbents.
Under conditions of 25 DEG C, 100KPa, the CH of products obtained therefrom4And N2Adsorbance is respectively 15.3cm3/ g and 3.3cm3/ G, the equilibrium separation ratio of methane nitrogen is 4.6.
Embodiment 3：
A kind of preparation method of the X-type molecular sieve of pressure swing adsorption/separation of methane nitrogen/LDHs compound adsorbents, including such as Lower step：
1) 150g Al (NO are weighed3)3·9H2O and 51.3g Mg (NO3)2·6H2O is dissolved in 1200mL deionized waters, is matched somebody with somebody It is 0.5molL that total concentration, which is made,-1Mixing salt solution, weigh 80g NaOH and be dissolved in 400ml deionized waters and be configured to 5mol·L-1NaOH solution, NaOH solution is added dropwise in mixing salt solution under agitation, during dropwise addition System pH is kept 9~10, NaOH solution continues stirring ageing 3 hours after being added dropwise, products therefrom is filtered, using going Ionized water is washed 3 times repeatedly, and it is 2wt% hydrotalcite colloidal sol to be placed in 6 hours obtained solid contents in 100 DEG C of thermostatic drying chambers；
2) weigh 0.1~1 μm of NaX type molecular sieves 50g and be added to the sodium lignin sulfonate water that 500ml concentration is 10g/L In solution, be initially positioned in 20Hz ultrasonic devices ultrasound 2 hours, after be placed under the conditions of 50 DEG C of stirred in water bath and react 10 hours, instead Centrifuged after having answered and remove unreacted sodium lignin sulfonate, obtain the X-type molecular sieve that surface carries negative electrical charge；
3) the X-type molecular sieve 20g of gained in step 2) is taken to be placed in the colloidal sol obtained by 600g steps 1), by the mixing of the two Thing carries out ion-exchange reactions under the conditions of being placed in 70 DEG C of stirred in water bath, filtering and washing after reacting 8 hours, dries, obtains X-type molecule Sieve/LDHs compound adsorbents.
Under conditions of 25 DEG C, 100KPa, the CH of products obtained therefrom4And N2Adsorbance is respectively 15.6cm3/ g and 3.3cm3/ G, the equilibrium separation ratio of methane nitrogen is 4.7.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.

Claims (4)

  1. A kind of 1. preparation method of the X-type molecular sieve of adsorbing separation methane nitrogen/LDHs compound adsorbents, it is characterised in that Comprise the following steps：
    1) LDHs preparation：It is 0.5mol/L that the magnesium salts of solubility and aluminium salt, which are placed in deionized water dissolving to be configured to total concentration, Solution A, aqueous slkali B is added dropwise in solution A under constant agitation, in the process keep solution ph 9~10, Aqueous slkali B continues stirring ageing 3~5 hours after being added dropwise, filtering, wash repeatedly to neutrality, products obtained therefrom is placed in 80~ Colloidal sol is made within 6~10 hours in 100 DEG C of baking oven；
    2) modification of X-type molecular sieve：By particle diameter 0.1~1 μm of NaX type molecular sieves be added to anionic polyelectrolyte or it is cloudy from In the aqueous solution of sub- surfactant, ultrasonication 1~3 hour, react 4 under the conditions of 50~70 DEG C of stirred in water bath ~10 hours, described anionic polyelectrolyte was the one or more in kayexalate, sodium lignin sulfonate, described Anion surfactant be neopelex, the water of the anionic polyelectrolyte or anion surfactant Solution concentration is 1g/L, and the NaX types molecular sieve is 1 with the weight ratio of anionic polyelectrolyte or anion surfactant： (0.01~0.03), centrifuged after having reacted and remove unreacted anionic polyelectrolyte or anion surfactant, obtained The X-type molecular sieve of negative electrical charge is carried to surface；
    3) preparation of X-type molecular sieve/LDHs compound adsorbents：The X-type molecular sieve of gained in step 2) is added obtained by step 1) Colloidal sol in, the weight ratio of NaX types molecular sieve and colloidal sol is 1：25, after the mixture of the two be placed in 50~60 DEG C of water-baths stirred Ion-exchange reactions is carried out under the conditions of mixing, in 6~8 hours reaction time, filtering and washing, dries, obtain X-type molecule after completion of the reaction Sieve/LDHs compound adsorbents.
  2. 2. the preparation method of compound adsorbent according to claim 1, it is characterised in that aluminium salt described in step 1) and magnesium Salt is aluminum nitrate and magnesium nitrate, and the aqueous slkali is sodium hydroxide solution.
  3. 3. a kind of preparation method according to any one of 1-2 prepares X-type molecular sieve/LDHs compound adsorbents of gained.
  4. 4. X-type molecular sieve according to claim 3/LDHs compound adsorbents are in pressure swing adsorption/separation of methane/nitrogen Using.
CN201711037930.4A 2016-03-31 2016-03-31 A kind of preparation method of the X-type molecular sieve of adsorbing separation methane nitrogen/LDHs compound adsorbents Pending CN107551994A (en)

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CN201711053602.3A Pending CN107694548A (en) 2016-03-31 2016-03-31 A kind of preparation method of the X-type molecular sieve of pressure swing adsorption/separation of methane nitrogen/LDHs compound adsorbents
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CN110038724A (en) * 2019-04-26 2019-07-23 江苏中科睿赛污染控制工程有限公司 A kind of gas purification dedusting module
CN112569898A (en) * 2019-09-30 2021-03-30 中国科学院大连化学物理研究所 Adsorbent and preparation method and application thereof
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