Preparation and application method of stepped pore molecular sieve for refining and separating phase change wax

An application method and molecular sieve technology, which are applied in the fields of petroleum wax refining, chemical instruments and methods, heat exchange materials, etc., can solve the problems of high isoparaffin content, low phase change enthalpy value, and no relevant reports, and reduce the The effect of isoparaffin content, reduction of energy consumption of equipment, and expansion of selection range

Active Publication Date: 2021-06-22
北京明星绿能化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Molecular sieve dewaxing process mostly uses 5A molecular sieve or modified 5A molecular sieve as adsorbent, which limits the composition of raw materials. The product has a wide carbon number distribution, high isoparaffin content, low adsorption and separation efficiency and low phase change enthalpy, and cannot solve high Adsorption and separation of normal alkanes with carbon number
However, there is no relevant report on the technology of distillation combined with high-silicon step-pore Beta molecular sieve as an adsorbent for refining and separating to prepare phase-change wax.

Method used

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  • Preparation and application method of stepped pore molecular sieve for refining and separating phase change wax
  • Preparation and application method of stepped pore molecular sieve for refining and separating phase change wax
  • Preparation and application method of stepped pore molecular sieve for refining and separating phase change wax

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Effect test

Embodiment 1

[0047] The present embodiment provides a kind of preparation method of Beta molecular sieve former powder, comprises the following steps:

[0048] Beta molecular sieve raw powder was synthesized according to the method disclosed in the example of US Patent No. 3,308,069. First add 0.10g NaAlO 2 (chemically pure, Al 2 o 3 , 41wt%) solid and 3.62g TEAOH solution (industrial grade, 20wt%) preparation solution, then add 3.28g silica sol (industrial grade, SiO 2 ≥ 30wt%), mix uniformly to form a gel, and the molar ratio of each material is: SiO 2 / Al 2 o 3 =40, Na 2 O / SiO 2 =0.004, TEA 2 O / SiO 2 =0.15,H 2 O / SiO 2 = 17.6, continue to stir for about 1 hour, put the prepared gel into a stainless steel reactor with a polytetrafluoroethylene liner, crystallize at 150 ° C for about 4 days, cool to room temperature, filter and wash.

[0049] The Beta molecular sieve former powder TEM photograph that embodiment 1 prepares sees figure 1 (a), the physical and chemical properties...

Embodiment 2

[0051] This embodiment provides a preparation method for the synthesis of a stepped pore Sec-SiBeta molecular sieve, comprising the following steps:

[0052] (1) Preparation of high silicon Si-Beta molecular sieve

[0053] Firstly, beta raw powder and ammonium chloride aqueous solution (2mol / L, 80°C) were ion-exchanged for 3 hours according to the solid-to-liquid ratio of 1:10, and the product was filtered and washed with deionized water and dried in an oven at 100°C for 24 hours; Prepare H-Beta zeolite by roasting in muffle furnace (air atmosphere, 560°C) for 4h to remove organic template; weigh 1.0g H-Beta zeolite and add 20mL HNO 3 Solution (pH=1.0, 13mol / L), stirred continuously at 100°C for 8h; the treated liquid was cooled to room temperature to filter out the acid solution, washed with deionized water until pH=6.0-7.0, filtered, dried at 100°C for 24h, the product was named Si -Beta.

[0054] (2) Secondary crystallization to synthesize step-pore Sec-SiBeta molecular s...

Embodiment 3

[0063] This embodiment provides a method for preparing a stepped pore Sec-SiBeta molecular sieve adsorbent, comprising the following steps:

[0064] Mix the original powder of stepped hole Sec-SiBeta molecular sieve, kaolin, bentonite and sage powder according to the mass ratio of 92:6:1:1, add an appropriate amount of water, the amount of water is 12wt% of the solid powder, after stirring evenly, extrude with a screw Extruded into rods with a diameter of 1.6mm, dried at 90°C for 8 hours, heated to 550°C at a rate of 2°C / min and roasted for 4 hours, and the above-mentioned molecular sieve crystals were prepared in 0.6mol / L CaCl 2 The solution was ion-exchanged twice at 90°C for 2 hours each time, washed with suction to neutrality, dried at 110°C for 24 hours, and activated at 450°C for 3 hours to obtain the Sec-SiBeta molecular sieve strip adsorbent with stepped pores.

[0065] A high-quality phase-change wax product is prepared with refinery-reduced second-line oil as a liqui...

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Abstract

The invention relates to the technical field of molecular sieve preparation and application, and particularly discloses a preparation method of a stepped pore molecular sieve for refining and separating phase change wax, wherein the preparation method comprises the following steps: step 1, weighing Beta molecular sieve raw powder, carrying out ammonium ion exchange, and roasting at high temperature to remove an organic template agent to obtain an H-Beta molecular sieve; step 2, carrying out acid treatment and dealumination on the H-Beta molecular sieve obtained in the step 1, and thus obtaining a Si-Beta molecular sieve with a certain T atom defect vacancy; and step 3, taking the Si-Beta molecular sieve subjected to dealumination in the step 2 as a Si source, and carrying out secondary crystallization through an organic template agent to obtain the stepped pore Sec-SiBeta molecular sieve with high silica-alumina ratio, high mesoporous pore volume and rich Si-OH. The defects in the prior art are overcome, and the prepared molecular sieve has the advantages of micropore-mesopore composite stepped structure, regular and ordered pore structure, fewer acid sites, water resistance, thermal stability and the like.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation and application, in particular to a preparation and application method of a step-pore molecular sieve used for refining and separating phase change wax. Background technique [0002] Phase change energy storage material is a kind of material that utilizes physical phase change at a certain temperature to realize energy (heat) storage and release. It is used in building heating, cold chain transportation, intelligent temperature-regulating fiber, temperature control of biological agents, new energy vehicles, temperature management of electronic components and other fields. Phase change paraffin (phase change wax) is mainly composed of normal alkanes (C n h 2n+2 ) composition, its chemical properties are stable, non-corrosive, and non-environmental pollution. Organic phase change wax can effectively avoid the supercooling phenomenon and phase separation phenomenon of inorganic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/18B01J20/28B01J20/30C09K5/06C10G73/42
CPCB01J20/186B01J20/28054B01J20/28014C09K5/063C10G73/42
Inventor 李江成李聪孟凡芳陈怀彪岳国
Owner 北京明星绿能化工科技有限公司
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