Sorbent of zeolite with carrying silver, preparation method and application thereof

A silver-loaded zeolite and adsorbent technology, applied in chemical instruments and methods, other chemical processes, separation/purification of carboxylic acid compounds, etc., can solve the corrosion of refining equipment, uneven distribution of coarse pores, and reduce the use efficiency of adsorbents and other problems, to achieve the effect of simple preparation method and high industrialization prospect.

Active Publication Date: 2009-07-08
SHANGHAI HUAYI ENERGY CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] U.S. Patents US 3,927,078, US 4,046,807, US 4,115,444, US 4,252,741, US 4,374,070, US 4,430,273, US 4,559,183, US 5,003,104, US 5,292,948 and European patents EP 8396, EP 87,869, EP 8396, 87,869 In the process, iodide participates in the reaction as a co-catalyst, so the product inevitably contains trace amounts of inorganic iodine, organic iodide and molecular iodine impurities. 05-301839 (BP company) and patent publication level 05-125011 (BP company) disclosed in the presence of rhodium / methyl iodide catalyst, methanol and (or) acetic acid and (or) acetic anhydride prepared by carbonylation of methyl acetate method, the existing problem is, always contain a small amount of iodide impurity in acetic acid or acetic anhydride after distillation
[0007] 2. Crude acetic anhydride, or the iodide concentration in the crude acetic anhydride / crude acetic acid mixture is too high, which will cause corrosion to the refining device, which is mentioned by Daicel
Due to the uneven distribution of the amorphous binder among the zeolite powder crystal grains in the adsorbent particles, the coarse pore size distribution between the zeolite crystal grains is uneven. Diffusion to the zeolite crystal grains also reduces the use efficiency of the adsorbent and affects the strength of the adsorbent

Method used

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  • Sorbent of zeolite with carrying silver, preparation method and application thereof
  • Sorbent of zeolite with carrying silver, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put 80 grams of acid-resistant base zeolite into a 50mL autoclave, and add 40ml of 0.5mol / L ion-exchange silver-carrying Ag + Solution (AgNO 3 solution), heated to 140°C, and the constant temperature time was 6 hours. After the ion exchange silver loading was completed, the adsorbent was taken out, washed with distilled water, and dried in an oven at 80°C. EDX analysis was performed on the ion-exchange silver-loaded adsorbent, and the results obtained are shown in Table 1:

[0039] Table 1

[0040] element content Al (mol%) 2.61 Si (mol%) 32.57 Ag (mol%) 2.75 Na(mol%) 0.27 O (mol%) 61.8 Ag / Al 1.05 SiO 2 / Al 2 o 3 25 Ag wt% 13.06

Embodiment 2

[0042] Put the acid-resistant zeolite adsorbent into the ion exchange column, the solid volume of the exchange column is 20mL, and the solution concentration is 0.1mol / L Ag + Solution (AgNO 3 Solution), continue to flow through the exchange column, the duration is 24 hours, the temperature is 80 ℃, and the flow velocity is 4 m / s. The EDX method is used to analyze the composition of the ion-exchange silver-loaded sorbent. The results obtained are shown in Table 2:

[0043] Table 2

[0044] element content Al (mol%) 2.87 Si (mol%) 31.07 Ag (mol%) 1.55 Na(mol%) 0.06 O (mol%) 64.45 Ag / Al 0.54 SiO 2 / Al 2 o 3 21.65 Ag wt% 7.8

Embodiment 3～11

[0046] Take by weighing the ion-exchange silver-loaded adsorbent 16g (about 20mL) that embodiment 2 obtains, carry out the test of removing trace inorganic iodide in the acetic anhydride product under the conditions listed in table 3 respectively in the ion-exchange column, after the test, B The analysis results of inorganic iodide content and silver content in the acid anhydride product are listed in Table 3, to prove that the ion-exchange silver-loaded adsorbent has a good effect on removing trace amounts of inorganic iodide in the acetic anhydride product.

[0047] table 3

[0048]

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PUM

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Abstract

The invention discloses a silver-loaded zeolite adsorbent, a preparation method and application thereof. The silver-loaded zeolite adsorbent of the present invention is a silver-loaded acid-resistant zeolite, and the weight content of the silver is 7-15%. The silver-loaded zeolite adsorbent can be used to remove trace amounts of iodide in acetic anhydride products. Said zeolite has structural pores of 10 oxygen member rings and 12 oxygen member rings, high strength, uniform distribution of coarse pores between zeolite crystal grains and good acid resistance. The zeolite is used as a substrate to carry silver to make an adsorbent of silver-carrying acid-resistant zeolite, which has high adsorption effect on iodide molecules of different molecular sizes, has high strength, high silver-carrying amount, and excellent pore distribution. The silver-loaded zeolite adsorbent of the present invention has a simple and convenient preparation method, can effectively remove inorganic and / or organic iodide and / or molecular iodine in the crude product of acetic anhydride, and has a high prospect of industrial implementation.

Description

technical field [0001] The invention relates to a silver-loaded zeolite adsorbent and the application of its preparation method, in particular to the application of removing trace iodide in acetic anhydride products. technical background [0002] Acetic anhydride is widely used in industry as an acetylating agent. In the United States, 95% of the production of acetic anhydride in Japan is used to produce cellulose acetate, triacetate cellulose containing 61.5-62% acetyl is used to manufacture high-strength, non-flammable photosensitive films, and diacetate containing 50-57% acetyl Cellulose is used to make cigarette filters and plastics. Acetic anhydride is also widely used in medicine, dyestuff, pesticide and fragrance industry. [0003] U.S. Patents US 3,927,078, US 4,046,807, US 4,115,444, US 4,252,741, US 4,374,070, US 4,430,273, US 4,559,183, US 5,003,104, US 5,292,948 and European patents EP 8396, EP 87,869, EP 8396, 87,869 In the process, iodide participates in the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/18C07C51/47C07C53/08
Inventor 陈墨庆周皓岚龙英才崔伟
Owner SHANGHAI HUAYI ENERGY CHEM
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