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Preparation method and preparation device of SSZ (sulfasalazine)-13 molecular sieve

A preparation device and technology of molecular sieve, which is applied in the field of preparation of SSZ-13 molecular sieve, can solve problems such as prone to abnormality, poor product performance stability, and low production efficiency, and achieve the effect of improving production efficiency and shortening the reaction cycle

Inactive Publication Date: 2019-02-12
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has a long reaction cycle, cumbersome equipment cleaning, low production efficiency, affects production capacity, and poor product performance stability; in order to increase production capacity and expand equipment volume, however, a large number of raw materials are simply put in at one time, and abnormalities are prone to occur during production, resulting in Difficult to handle, increased costs, huge losses

Method used

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  • Preparation method and preparation device of SSZ (sulfasalazine)-13 molecular sieve
  • Preparation method and preparation device of SSZ (sulfasalazine)-13 molecular sieve
  • Preparation method and preparation device of SSZ (sulfasalazine)-13 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 Preparation of SSZ-13 molecular sieve

[0035] Proceed as follows:

[0036] 1.1 Add 7.958 kg of water into the glass water bath and add 0.168 kg of aluminum hydroxide, 0.084 g of sodium hydroxide, 2.400 kg of N,N,N-trimethyl-1-amantadine, and 0.060qw of seed crystals at one time while stirring kilogram;

[0037] Among them, the addition of each raw material was stirred for 10 minutes; after adding seed crystals and stirring for 1 hour, 1.952 kg of silica was added;

[0038] After stirring for 1 hour, heat up to 60°C and stir at 60°C for 6 hours to form a jelly; transport the jelly to the buffer storage tank for synthesis;

[0039] 1.2 Start the continuous synthesis reactor:

[0040] Set the flow rate of the pure water metering pump to 1000ml / min; set the pure water preheating tube temperature of the tubular super (sub)critical reactor to 270°C; the reaction mixer 290°C, the synthesis section temperature 290°C, and the set outlet temperature 130°C , Test run with pure w...

Embodiment 2

[0045] Example 2 Preparation of a SSZ-13 molecular sieve

[0046] Proceed as follows:

[0047] 2.1 Add 10.974 kg of water to the glass water bath, and under stirring, add 0.736 kg of sodium metaaluminate, 0.147 kg of sodium hydroxide, 5.206 kg of N,N,N-trimethyl-1-amantadine, and 0.152 kg of seed crystals. , The addition of each raw material is stirred for 10 minutes; add seed crystals and stir for 1 hour, then add 5.010 g of silica; stir for 1.5 hours and heat up to 80°C, stir at 80°C for 12 hours to form a jelly; transport the jelly To the buffer storage tank to prepare for synthesis;

[0048] 2.2 Start the continuous synthesis reactor:

[0049] Set the flow rate of the pure water metering pump to 1500ml / min; set the pure water preheating tube temperature of the tubular super (sub)critical reactor to 330°C; the reaction mixer 340°C, the synthesis section temperature 350°C, and the set outlet temperature 130°C , Test run with pure water (instead of the initial mixture), adjust the ...

Embodiment 3

[0054] Example 3 Preparation of a SSZ-13 molecular sieve

[0055] Proceed as follows:

[0056] 3.1 Add 15.85 kg of sodium to a glass water bath kettle, add 3.156 kg of aluminum sulfate, 1.928 kg of sodium hydroxide, 6.506 kg of N,N,N-trimethyl-1-amantadine, 0.200 kg of seed crystals at one time under stirring. Add the raw materials and stir for 10 minutes at intervals; add seed crystals and stir for 2 hours, then add 5.856 kg of silica; stir for 2 hours and heat up to 90℃, stir at 90℃ for 8 hours to form a jelly; transport the jelly to the buffer The storage tank is ready for synthesis;

[0057] 3.2 Start the continuous synthesis reactor:

[0058] Set the flow rate of the pure water metering pump 2000ml / min; set the temperature of the pure water preheating tube of the tubular super (sub)critical reactor to 360°C; the reaction mixer 380°C, the synthesis section temperature 380°C, and the set outlet temperature 130°C , Test run with pure water (instead of the initial mixture), adjust ...

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Abstract

The invention relates to a preparation method and a preparation device of an SSZ (sulfasalazine)-13 molecular sieve. The preparation method of the SSZ-13 molecular sieve comprises the step that sol issubjected to a super / sub critical reaction. The preparation device comprises a material mixing unit, a synthesizing unit, a cooling unit and a discharging control unit which are connected sequentially, wherein the material mixing unit is connected with a pure water pre-heating pipe and a sol output pipe respectively. Continuous tubular super (sub) critical liquid phase synthesizing equipment is utilized to prepare the SSZ-13 molecular sieve, not only can the reaction period be shortened, and the production efficiency is improved; but also the problems that too much raw materials are added atonce, thus abnormal conditions occur on production, and the cost is increased can be avoided.

Description

Technical field [0001] The invention relates to a preparation method of SSZ-13 molecular sieve and a preparation device thereof, and belongs to the technical field of molecular sieve preparation. Background technique [0002] SSZ-13 molecular sieve is a molecular sieve with CHA topology, and its conventional preparation method mainly adopts batch reaction. However, this method has a long reaction cycle, cumbersome equipment cleaning, low production efficiency, affecting productivity, and poor product performance stability; in order to increase production capacity and expand the equipment volume, but simply put a lot of raw materials at one time, abnormalities are prone to occur in production, resulting in Difficulty in handling, increased costs, and huge losses. Summary of the invention [0003] The invention provides a method for preparing SSZ-13 molecular sieve by using continuous tubular super (sub)critical liquid phase synthesis equipment, which greatly shortens the reaction ...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B37/00
CPCC01B37/005C01B39/04
Inventor 宋锡滨董成利艾辽东焦英训潘光军
Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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