Low-temperature preparation method of lithium slag based NaA molecular sieve

A molecular sieve and low-temperature technology, which is applied in the direction of A-type crystalline aluminosilicate zeolite and crystalline aluminosilicate zeolite, etc., can solve problems such as poor controllability, long reaction time, unfavorable economic benefit improvement and environmental protection, etc., to avoid Effect of nucleation and improvement of synthesis purity

Active Publication Date: 2019-03-19
CHINA UNIV OF MINING & TECH (BEIJING)
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Problems solved by technology

At present, fly ash is mostly used in the synthesis of NaA zeolite from industrial solid waste, and the lithium slag has not been fully utilized. Moreover, the synthesis temperature of NaA molecular sieve using other solid waste to synthesize NaA molecular sieve is mostly at 90-120°C, and the energy consumption is high. It is not conducive to the improvement of economic benefits of enterprises and environmental protection. There are also a small number of NaA molecular sieves synthesized at room temperature, but generally pure chemical reagents are used, and the reaction time is too long (2 to 7 days), and the controllability is poor. At present, lithium slag is basically not used. Or other industrial solid wastes below 80 ℃ and a precedent for preparing NaA molecular sieves in a short period of time

Method used

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  • Low-temperature preparation method of lithium slag based NaA molecular sieve

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preparation example Construction

[0026] The invention provides a low-temperature preparation method of lithium slag-based NaA molecular sieve, comprising the following steps:

[0027] (1) Carry out pretreatment to raw material lithium slag;

[0028] (2) Alkali melting is carried out to the pretreated lithium slag by using an alkali melting agent to obtain silicate clinker;

[0029] (3) adding an aluminum source and a water source to the silicate clinker, adjusting the molar ratio of silicon to aluminum to 1.0 to 2.4:1 and the molar ratio of water to alkali to 40 to 80:1 to obtain a NaA molecular sieve precursor; the silicon Al molar ratio to SiO 2 and Al 2 o 3 In terms of the amount of substance, the molar ratio of water to alkali is expressed in H 2 O and Na 2 A measure of the substance of O;

[0030] (4) The NaA molecular sieve precursor is subjected to a hydrothermal reaction at 45-75° C. to obtain a lithium slag-based NaA molecular sieve.

[0031] The invention pretreats the raw material lithium sl...

Embodiment 1

[0043] According to the reaction condition of table 1, take lithium slag 5g (containing SiO 2 :58.27wt%, Al 2 o 3 : 23.75wt%, SO 3 :9.06wt%, CaO: 5.81wt%, Fe 2 o 3 : 1.36wt%, other 1.75wt%, main crystalline phase is gypsum, quartz and spodumene), be pulverized to 200 orders, water eluting acid; Add solid sodium hydroxide 7.5g, make alkali-silicon mol ratio (Na 2 O / SiO 2 ) is 1.9, mix well and grind quickly. Alkali-melt the uniformly mixed raw materials at 600°C for 4 hours to obtain silicate clinker; grind the clinker until there is no graininess, add 6.05g NaAlO 2 , the SiO in the clinker 2 / Al 2 o 3 Molar ratio is adjusted to 1.0, then adds 130.66g deionized water, makes water / alkali mol ratio (H 2 O / Na 2 O) reached 56 to obtain the NaA molecular sieve precursor; stirred and aged at room temperature for 12 hours to obtain the reaction material; transferred the reaction material to the reaction kettle, crystallized at 60°C for 8 hours, and washed the product repeat...

Embodiment 2～12

[0047] The reaction steps are the same as in Example 1, and the reaction conditions are shown in Table 1.

[0048] XRD test and SEM observation were carried out on the products finally obtained in Examples 2-12, and the results are shown in Table 1.

[0049] The reaction condition and product of table 1 embodiment 1~12

[0050]

[0051] As can be seen from the results in Table 1, the present invention can obtain NaA molecular sieve at a low temperature of 45-75°C by controlling the reaction conditions, which significantly reduces the temperature of the hydrothermal reaction; in addition, the hydrothermal reaction time of the present invention is only 2-2 24h, which is much shorter than the reaction time at room temperature (2-7 days), and the obtained NaA molecular sieve crystallizes well, and no sodalite appears.

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Abstract

The invention provides a low-temperature preparation method of a lithium slag based NaA molecular sieve and belongs to the technical fields of industrial solid waste recycling and molecular sieve preparation. The low-temperature preparation method comprises the following steps: (1) pre-treating raw lithium slag; (2) performing alkali fusion on the pretreated lithium slag by adopting an alkali fusion agent so as to obtain silicate clinker; (3) adding an aluminum source and a water source into the silicate clinker, regulating the silicon-aluminum molar ratio to be (1.0-2.4):1 and controlling a water-alkali molar ratio to be (40-80):1 so as to obtain a NaA molecular sieve precursor; and (4) carrying out a hydrothermal reaction on the NaA molecular sieve precursor at a temperature of 45-75 DEGC, thereby obtaining the lithium slag based NaA molecular sieve. According to the preparation method disclosed by the invention, the lithium slag serves as the raw material, the high-purity lithium slag based NaA molecular sieve can be prepared at a low hydrothermal temperature in short reaction time, and high value-added utilization of the lithium slag is realized.

Description

technical field [0001] The invention relates to the technical field of industrial solid waste resource treatment and molecular sieve preparation, in particular to a low-temperature preparation method of lithium slag-based NaA molecular sieve. Background technique [0002] Lithium slag is the solid waste produced during the production of industrial lithium carbonate by the spodumene sulfuric acid method. The production of 1 ton of lithium carbonate products requires nearly 10 tons of lithium slag. my country is the country with the largest reserves of spodumene concentrate in the world, and Xinjiang and Sichuan are the main production bases of lithium salt. A large amount of lithium slag is disposed of by landfill or open-air stacking, which not only occupies land resources, but also pollutes air and water resources, posing a serious threat to the environment. Therefore, it is imminent to realize the high value-added utilization of lithium slag, and it is urgent to open up ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14
CPCC01B39/14C01P2002/72C01P2004/03C01P2004/61C01P2004/62
Inventor 刘泽李丽王吉祥李斯琦
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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