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Preparation method of amino modified layered double hydroxide

A technology of hydroxide and amino modification, applied in chemical instruments and methods, aluminum compounds, separation methods, etc., to achieve high utilization rate, increase adsorption capacity, and environmental friendliness

Inactive Publication Date: 2019-04-19
ZHEJIANG UNIV OF TECH
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  • Description
  • Claims
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Problems solved by technology

[0006] In order to overcome that the existing amino modification methods cannot meet the requirements of higher CO 2 To meet the requirements of adsorption performance, good economy and environmental friendliness, the present invention provides an ultrasonic-assisted one-step amino modification method to prepare CO 2 Amino-modified layered double hydroxides with promising adsorption applications

Method used

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  • Preparation method of amino modified layered double hydroxide
  • Preparation method of amino modified layered double hydroxide
  • Preparation method of amino modified layered double hydroxide

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preparation example Construction

[0021] refer to Figure 1 ~ Figure 3 , a preparation method of amino-modified layered double hydroxide, comprising the following steps:

[0022] (1) Dissolve 2.0-5.0g of anionic surfactant and 5.0-7.0g of aminosilane in 150mL of alcoholic water (V 无水乙醇 :V 去离子水 =1:2) obtain solution A; Magnesium nitrate hexahydrate and aluminum nitrate nonahydrate are prepared 50~100mL solution B according to the molar ratio of 3:1;

[0023] (2) Solution B was added dropwise to solution A at a rate of 0.5-1.0mL / min, and at the same time, the ultrasonic cell pulverizer was turned on to ultrasonicate the solution. The frequency was 5s on, 5s off, and the solution was continuously stirred during the dropping process to maintain the pH =10±0.1;

[0024] (3) After the solution B is added dropwise, turn off the ultrasonic cell breaker, age at 60-80° C. for 4-6 hours, filter with suction, wash and dry to obtain the amino-modified layered double hydroxide.

[0025] Further, the anionic surfactant u...

Embodiment 1

[0036] To 150mL (V 无水乙醇 :V 去离子水 =1:2) Add 2.83g sodium dodecylsulfonate and 6.94g N-aminoethyl-γ-aminopropyltrimethoxysilane to the aqueous alcohol solution to obtain solution A; take 3.99g magnesium nitrate hexahydrate and 1.95g Prepare 50mL nitrate aqueous solution B with aluminum nitrate nonahydrate; add solution B dropwise to solution A at a rate of 0.5mL / min, where n Mg :n Al :n 十二烷基磺酸钠 :n 氨基硅烷 =3:1:2:6, keep pH=10±0.1; after the dropwise addition, age at 75°C for 4h; filter, wash, and dry to obtain an amino-modified layered dihydrogen intercalated with an anionic surfactant oxide, its CO 2 The adsorption capacity was 1.11 mmol / g.

Embodiment 2

[0038] To 150mL (V 无水乙醇 :V 去离子水 =1:2) Add 2.83g sodium dodecylsulfonate and 6.94g N-aminoethyl-γ-aminopropyltrimethoxysilane to the aqueous alcohol solution to obtain solution A; take 3.99g magnesium nitrate hexahydrate and 1.95g Prepare 50mL nitrate aqueous solution B with aluminum nitrate nonahydrate; add solution B dropwise to solution A at a rate of 0.5mL / min, where n Mg :n Al :n 十二烷基磺酸钠 :n 氨基硅烷 =3:1:2:6, keep pH=10±0.1, insert the horn of the ultrasonic cell pulverizer into the solution during the co-precipitation process, the ultrasonic power is 65W, every work is 5s, and the interval is 5s; Turn off the ultrasound, and age the solution at 75°C for 4 hours; filter, wash, and dry to obtain an amino-modified layered double hydroxide intercalated with an anionic surfactant, whose CO 2 The adsorption capacity was 1.55 mmol / g.

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Abstract

The invention relates to a preparation method of amino modified layered double hydroxide, which comprises the following steps: (1) weighing and dissolving 2.0-5.0g of anionic surfactant and 5.0-7.0g of aminosilane in 150mL of alcohol aqueous solution to obtain solution A; preparing 50-100mL of solution B from magnesium nitrate hexahydrate and aluminum nitrate nonahydrate according to a molar ratioof 3.1; (2) dripping the solution B into the solution A at the speed of 0.5-1.0mL / min, starting an ultrasonic cell crusher to carry out ultrasonic treatment on the solution at the same time, whereinthe frequency is 5s, stopping the ultrasonic treatment for 5s, continuously stirring the solution in the dropping process, and keeping the pH value equal to 10+ / -0.1; and (3) after the dripping of thesolution B is finished, closing the ultrasonic cell crusher, aging for 4 to 6 hours at the temperature of between 60-80 DEG C, performing suction filtration, washing and drying to obtain the amino modified layered double hydroxide. According to the invention, the amino-modified layered double hydroxide with better CO2 adsorption application prospect is prepared.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic compounds, and in particular relates to a preparation method of an amino-modified layered double hydroxide compound. technical background [0002] Adsorption and capture of greenhouse gas CO by solid materials 2 The technology has the advantages of low energy consumption, low corrosion, wide application temperature, long service life, simple process flow, high degree of automation and no secondary environmental pollution, etc., and has great development prospects. [0003] Layered double hydroxide (LDH) is a layered inorganic functional material with more basic sites on the surface and a larger specific surface area, and has been used to adsorb and capture greenhouse gases. CO 2 . CO capture by layered double hydroxide adsorption 2 It has the advantages of high adsorption selectivity, wide range of adsorption temperature, fast adsorption and desorption rate, and no secondary pollution t...

Claims

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Application Information

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IPC IPC(8): B01J20/04B01J20/30B01D53/02C01F7/00C01F7/784
CPCB01D53/02B01J20/0248B01J20/041B01D2257/504C01F7/78Y02C20/40C01F7/784
Inventor 艾宁赵雨刘秋平王祁宁蒋益波楼洒
Owner ZHEJIANG UNIV OF TECH
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