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HMCM-49 molecular sieve production method

A HMCM-49, production method technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of incomplete recovery of hexamethyleneimine, direct discharge of hexamethyleneimine waste water, etc., and save equipment investment , the effect of reducing emissions

Active Publication Date: 2013-06-05
PETROCHINA CO LTD
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Problems solved by technology

[0004] Chinese patent 02145237.7 proposes a preparation method of MCM-49 molecular sieve, which circulates part of the mother liquor and recovers part of the remaining hexamethyleneimine, but does not completely recover hexamethyleneimine and completely solve the problem of hexamethyleneimine The problem of direct discharge of amine wastewater

Method used

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  • HMCM-49 molecular sieve production method

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Embodiment 1

[0013] Add 100kg of desalted water, 110kg of mother liquor, 11kg of sodium metaaluminate or sodium aluminate, 250kg of silica sol with a mass content of 26%, 35kg of hexamethyleneimine and 2kg of NaMCM-49 molecular sieves in sequence, and fully stir to carry out Batching, gelling and crystallization; at 40°C, enter the plate and frame filter press to separate the mother liquor. The mother liquor is poured into the mother liquor storage tank with a mother liquor pump; the filter cake is sent to the oxidation tank, and 90kg of desalted water is added, and 15kg of hydrogen peroxide with a mass content of 30% is added at 65°C, and oxidized for 5 hours; after the oxidation is completed, it is sent to a plate and frame filter press , 80kg of filtrate is discharged waste water; the filter cake is sent to the oven and dried at 120°C for 6 hours; after drying, it is roasted at 550°C for 8 hours to produce a small amount of waste gas; The aqueous citric acid solution with a mass content...

Embodiment 2

[0015] 70kg of desalted water, 150kg of mother liquor, 11Kg of sodium metaaluminate or sodium aluminate, and 250kg of silica sol with a mass content of 26%. 35kg of hexamethyleneimine and 2kg of NaMCM-49 molecular sieve are added in turn, and fully stirred for batching, gelation and crystallization; at 60°C, enter the plate and frame filter press to separate the mother liquor, and use the mother liquor pump to pump the mother liquor Put the filter cake into the mother liquor storage tank; send the filter cake to the oxidation tank, add 120kg of desalted water, add 20kg of hydrogen peroxide with a mass content of 30% at 65°C, and oxidize for 4 hours; Drainage water; the filter cake is sent to an oven and dried at 120°C for 10 hours; roasted at 540°C for 20 hours to produce a small amount of waste gas; after cooling, put it into a pulping tank and add citric acid aqueous solution with a mass content of 6% , sent to the rotary vane dynamic filter press, washed for 30min, and test...

Embodiment 3

[0017] Add 100kg of desalted water, 110kg of mother liquor, 11Kg of sodium metaaluminate or sodium aluminate, 250kg of silica sol with a mass content of 26%, 35kg of hexamethyleneimine and 2kg of NaMCM-49 molecular sieves in sequence, and fully stir to carry out Batching, gelling and crystallization; at 50°C, enter the plate and frame filter press to separate the mother liquor. The mother liquor is poured into the mother liquor storage tank with a mother liquor pump; the filter cake is sent to the oxidation tank, and 200kg of desalted water is added, and at 65°C, 30kg of hydrogen peroxide with a mass content of 30% is added, and oxidized for 5 hours; after the oxidation is completed, it is sent to a plate and frame filter press , 160kg of filtrate is discharged waste water; the filter cake is sent into the oven and dried for 6h at 120°C; roasted for 15h at 560°C to produce a small amount of waste gas; after cooling, put it into the pulping tank and add 15 % citric acid aqueous...

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Abstract

The present invention relates to a HMCM-49 molecular sieve production method, which comprises: adopting silica sol, sodium aluminate or sodium aluminate, hexamethyleneimine, desalted water, hydrogen peroxide and citric acid as raw materials, and carrying out material preparing, gelatinizing and crystallization in a reaction kettle; adopting a plate and frame filter press to separate a mother liquor to be recycled; adding the desalted water to filter cake, adopting hydrogen peroxide to carry out oxidation, cooling, and adopting a 5-20% citric acid aqueous solution to carry out pulping; and adopting a spiral vane type dynamic filter press to carry out washing and exchanging, and carrying out drying and roasting to obtain the HMCM-49 molecular sieve, wherein the liquid portion is subjected to evaporation and condensation to be adopted as the desalted water so as to be recycled. According to the present invention, the wastewater emission amount is 1 / 20 of the wastewater emission amount of the traditional process, the waste gas emission amount is 1 / 2-1 / 3 of the waste gas emission amount of the traditional process, and the solid sodium citrate waste can be used in a degradation manner.

Description

Technical field: [0001] The invention relates to a production method of HMCM-49 molecular sieve, in particular to a production method of HMCM-49 molecular sieve with less waste water discharge and less waste gas discharge. Background technique: [0002] HMCM-49 molecular sieve is the direct raw material for the preparation of HMCM-49 catalyst. It is gelled and crystallized by silica sol, sodium aluminate (or sodium metaaluminate) aqueous solution and hexamethyleneimine, and the mother liquor is separated to produce NaMCM. -49 molecular sieve, exchanged with ammonium nitrate aqueous solution, dried and roasted to produce HMCM-49 molecular sieve. [0003] At present, in the production of HMCM-49 molecular sieve, in the process of gelation and crystallization, the reaction is carried out in aqueous solution, and a certain amount of unreacted hexamethyleneimine is directly entered into the mother liquor, usually the mother liquor is directly used as waste water. Discharge, beca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 邓广金肖冰赵胤李正崔龙周玮焦凤茹张钰
Owner PETROCHINA CO LTD
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