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Preparation method of clay base gasoline desulfurization adsorbent

A technology of adsorbent and clay, which is applied in the field of clay-based desulfurization adsorbent, and can solve problems such as complex preparation process

Active Publication Date: 2015-07-08
江苏纳欧新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention overcomes the disadvantages of complex preparation process of desulfurization adsorbent in the prior art, and provides a preparation method of clay-based gasoline desulfurization adsorbent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Add 5g halloysite into 31.25mL titanium tetrachloride and titanium sulfate mixed solution, the molar ratio of titanium sulfate and titanium tetrachloride is 0.1:1, Ti 4+ The solubility is 1mol / L, soaked for 2 hours, heated to 90°C, kept warm and crystallized for 2 hours, and adjusted the pH to about 6-7 with 0.5mol / L NaOH solution to obtain TiO 2 / Modified clay composite dispersion.

[0028] 2. While stirring, add 250 mL of deionized water and 1.25 g of CuSO to the composite dispersion obtained in step 1 4 ·5H 2 O and 2.5g methanol, placed under sunlight for 1 hour, filtered, washed, and dried to obtain Cu 2 O / TiO 2 / Modified clay composite desulfurization adsorbent.

[0029] The XRD test shows that the grain size of anatase in titanium dioxide is 6.6nm, Cu 2 The grain size of O is 3.7 nm. BET test results: halloysite specific surface 42.92m 2 / g, pore volume 0.13cm 3 / g; Composite adsorbent specific surface area 48.27m 2 / g, pore volume 0.16cm 3 / g.

[00...

Embodiment 2

[0032] 1. Add 5g of bentonite to 41.67mL of titanium tetrachloride and titanium sulfate mixed solution, the molar ratio of titanium sulfate to titanium tetrachloride is 1:1, Ti 4+ The solubility is 3mol / L, soaked for 4 hours, heated to 120°C, kept warm for 4 hours to crystallize, and adjusted the pH to about 6-7 with 3mol / L KOH solution to obtain TiO 2 / Modified clay composite dispersion.

[0033] 2. Add deionized water 1000mL, 10.87gCu(NO 3 ) 2 ·3H 2 O and 43.48g of isopropanol were placed under sunlight for 8 hours, filtered, washed, and dried to obtain Cu 2 O / TiO 2 / Modified clay composite desulfurization adsorbent.

[0034] The XRD test shows that the grain size of anatase in titanium dioxide is 9.3nm, Cu 2 The grain size of O is 5.7 nm. BET test results: bentonite specific surface 179.23m 2 / g, pore volume 0.24cm 3 / g; composite adsorbent specific surface 186.27m 2 / g, pore volume 0.27cm 3 / g.

[0035] The measured sulfur content of the simulated gasoline afte...

Embodiment 3

[0037] 1. Add 5g of attapulgite clay to 39.07mL of titanium tetrachloride and titanium sulfate mixed solution, the molar ratio of titanium sulfate to titanium tetrachloride is 0.5:1, Ti 4+ The solubility is 2mol / L, soaked for 3 hours, heated to 105°C, kept warm and crystallized for 3 hours, adjusted the pH to about 6-7 with 1.75mol / L ammonia water, and obtained TiO 2 / Modified clay composite dispersion.

[0038] 2. Add deionized water 625mL, 5gCu(CH 3 COO) 2·H 2 O and 15g ethylene glycol, placed under sunlight for 4 hours, filtered, washed, and dried to obtain Cu 2 O / TiO 2 / Modified clay composite desulfurization adsorbent.

[0039] The XRD test shows that the grain size of anatase in titanium dioxide is 8.1nm, Cu 2 The grain size of O is 4.9 nm. BET test results: attapulgite clay specific surface 123.42m 2 / g, pore volume 0.48cm 3 / g; Composite adsorbent specific surface 135.17m 2 / g, pore volume 0.53cm 3 / g.

[0040] The measured sulfur content of the simulated g...

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PUM

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Abstract

The invention overcomes the shortcoming of complexity of a desulfurization adsorbent preparation process in the prior art, and provides a preparation method of a clay base gasoline desulfurization adsorbent. The preparation method includes the steps: adding clay into mixed solution of titanium tetrachloride and titanium sulfate, dipping the clay at the room temperature, increasing the temperature to crystallization temperature and adding alkali solution for adjusting pH (potential of hydrogen) to obtain TiO2 / modified clay complex dispersion liquid; adding deionized water, copper salt and alcohol into the dispersion liquid under the condition of stirring, irradiating the dispersion liquid in the sun and filtering, washing and drying the dispersion liquid to obtain Cu2O / TiO2 / modified clay complex desulfurization adsorbent. The mixed solution of titanium salt can generate high-concentration mixed acid in hydrolysis, the clay can be more effectively acidized and activated, the specific surface area and the pore volume of the clay are increased, the number of silicon hydroxyls on the surface of the clay is increased, and deposition of active component particles is facilitated. Anatase type nano-titania with a smaller gain size can be generated on the surface of the clay by the aid of negative ions generated by the mixed solution of the titanium salt.

Description

technical field [0001] The invention belongs to the field of gasoline desulfurization and relates to a clay-based desulfurization adsorbent with high selectivity for thiophene sulfur compounds in gasoline. Background technique [0002] SO produced by combustion of sulfur compounds in gasoline x Severe pollution of the atmosphere is also one of the main reasons for the formation of haze weather. At the same time, sulfides can also corrode the engine and reduce the service life of the engine. Many countries in the world have proposed increasingly stringent standards and regulations on the sulfur content in gasoline. Among them, the European Union stipulates that the sulfur content in gasoline must not exceed 10ppm, and Japan and the United States also limit the sulfur content in gasoline to less than 15ppm. In my country, only Beijing, Shanghai and other regions have realized the sales of National V gasoline (sulfur content <10ppm), and the gasoline sold in most areas has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/12B01J20/30C10G25/00
Inventor 姚超王桐左士祥马建锋刘文杰魏科年李霞章李为民
Owner 江苏纳欧新材料有限公司