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Silver-carried big-hole zeolite molecular sieve adsorbent, its preparing method and use

A technology of zeolite molecular sieve and large-pore zeolite, which is applied in chemical instruments and methods, other chemical processes, etc., can solve a wide range of adsorbents that are not involved and its reactivation, uneven distribution of coarse pores and pore size, and reduce the efficiency of adsorbent use. and other problems, to achieve the effect of high industrialization implementation prospects, large iodine removal capacity, and high strength

Inactive Publication Date: 2007-06-13
SHANGHAI HUAYI ENERGY CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the presence of rhodium / methyl iodide catalyst disclosed in Japanese patent patent publication level 07-215909 (Dacel Corporation), patent publication level 05-301839 (BP company) and patent publication level 05-125011 (BP company), methanol and ( Or) the method of acetic acid and (or) acetic anhydride prepared by methyl acetate carbonylation, existing problem is, always contain a small amount of iodide impurity in acetic anhydride or acetic acid after distillation
[0007] 2. If the concentration of iodide in crude acetic anhydride or crude acetic anhydride / crude acetic acid mixture is too high, it 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, and there is no description of the level that can reduce the total iodine content in acetic acid
[0012] Patent CN 1207093C discloses the preparation method and application of high silver-loaded zeolite molecular sieve adsorbent modified by natural zeolite. The silver-loaded amount reaches 26%. Patent CN 1201859C discloses a high-loaded Silver content ZSM-5 zeolite deiodination adsorbent, the silver loading can reach up to 20%. The above two patents only involve the removal of organic iodide in acetic acid, and do not involve the wider range of use of the adsorbent and its reactivation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 80 grams of large-pore zeolite molecular sieve adsorbent into the ion exchange column, the solid volume of the exchange column is 100mL, and the solution concentration is 1mol / L Ag + Solution (AgNO 3Solution), continuously flow through the exchange column, the duration is 24 hours, the temperature is 100 ℃, the liquid hourly space velocity (LHSV) is 4h -1 , using the EDX method to analyze the composition of the ion-exchange silver-loaded adsorbent, the results obtained are shown in Table 1:

[0031] Table 1

[0032] the element

Embodiment 2

[0034] Put 80 grams of macroporous molecular sieve zeolite molecular sieve adsorbent into the ion exchange column, the solid volume of the exchange column is 100mL, 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 60 ° C, and the flow rate is 6 hours of liquid hourly space velocity -1 , using the EDX method to analyze the composition of the ion-exchange silver-loaded adsorbent, the results obtained are shown in Table 2:

[0035] Table 2

[0036] the element

Embodiment 3～11

[0038] Take by weighing the fresh ion-exchange silver-loaded adsorbent 16g (about 20mL) that embodiment 1 obtains, carry out the test of removing trace iodide in the acetic anhydride product under the conditions listed in table 3 respectively in the ion-exchange column, after the test The analysis results of inorganic iodide content and silver content in the acetic 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.

[0039] table 3

[0040]

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PUM

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Abstract

The present invention discloses a silver-carrying macroporous zeolite molecular sieve adsorbent, its preparation method and application. The basis used by the invented silver-carrying macroporous zeolite molecular sieve adsorbent is a kind of macroporous zeolite molecular sieve with good macroporous channel distribution, its average pore size is 11 nm, and its pore structure is uniform. The silver weight content of silver-carrying macroporous zeolite molecular sieve adsorbent made up by utilizing silver salt solution cation exchange is 10-18%. For inorganic or organic iodides with different molecular sizes and molecular iodine said adsorbent has high adsorption action, and its strength is high.

Description

technical field [0001] The invention relates to a silver-loaded large-pore zeolite molecular sieve adsorbent and its preparation method and application, in particular to the application of removing trace amounts of iodide in acetic anhydride products. Background technique [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 ...

Claims

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Application Information

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IPC IPC(8): B01J20/18B01J20/32
Inventor 周皓岚陈墨庆崔伟李俊岭周亚明龙英才
Owner SHANGHAI HUAYI ENERGY CHEM
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