RU1610777C - Method of preparing high-silicon zeolite type zsm-5 - Google Patents

Method of preparing high-silicon zeolite type zsm-5 Download PDF

Info

Publication number
RU1610777C
RU1610777C SU4366373A RU1610777C RU 1610777 C RU1610777 C RU 1610777C SU 4366373 A SU4366373 A SU 4366373A RU 1610777 C RU1610777 C RU 1610777C
Authority
RU
Russia
Prior art keywords
water
aluminium
silicon
product
zeolite
Prior art date
Application number
Other languages
Russian (ru)
Inventor
Л.Д. Коновальчиков
И.Е. Горбаткина
Б.К. Нефедов
Т.В. Алексеева
О.Д. Коновальчиков
Г.Д. Чукин
Б.Л. Хусид
Н.Н. Ростанин
О.А. Конакова
А.М. Зубков
Ю.Н. Зеленцов
Original Assignee
Всесоюзный научно-исследовательский институт по переработке нефти
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Всесоюзный научно-исследовательский институт по переработке нефти filed Critical Всесоюзный научно-исследовательский институт по переработке нефти
Priority to SU4366373 priority Critical patent/RU1610777C/en
Application granted granted Critical
Publication of RU1610777C publication Critical patent/RU1610777C/en

Links

Images

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

FIELD: chemical technology. SUBSTANCE: silicon-containing reagent (sodium silicate, silicon sol, silica gel, aerosil) is mixed with aluminium-containing reagent (sodium aluminate, aluminium hydroxide, aluminium salts), alkaline metal hydroxide, aliphatic amine or diamine, or triamine or aminoalcohol, neutral water-soluble organic compound (glycerol or ethylene glycol, or diethylene glycol, or ethanol, or isopropanol, or isobutanol, or methylethylketone) and water in capacity with mixer. Prepared gel is homogenized by stirring at the room temperature for 0.5 h, placed into autoclave made of stainless steel and crystallized at 130-180 C. Mole ratio of neutral water-soluble organic compound and water (0.005-0.051):1. After termination of crystallization stage reaction mixture is cooled slowly at the rate 5-10 C/h up to 50 C, then zeolite is filtered off, washed with distilled water up to pH 8-9 and dried at 120 C for 6-10 h. Prepared zeolite is ZSM-5 type. Method is used in oil processing and petrochemical industry. EFFECT: increased crystallinity of product. 1 tbl

Description

Изобретение относится к способам получения высококремнеземного цеолита типа ZSM-5, применяемого в качестве компонента катализаторов и сорбентов в нефтеперерабатывающей и нефтехимической промышленности. The invention relates to methods for producing high-silica zeolite type ZSM-5, used as a component of catalysts and sorbents in the oil refining and petrochemical industries.

Целью изобретения является повышение степени кристалличности продукта. The aim of the invention is to increase the degree of crystallinity of the product.

П р и м е р. Готовят реакционную смесь со следующим мольным соотношением ингpедиентов: Na2O 50 МЭА 53 C8H3O Al2O3 50 SiO2 535 H2O, где МЭА моноэтаноламин, для чего к 254 мл дистиллированной воды приливают 6,31 мл раствора алюмината натрия (Na2O 272,8 г/л, Al2O3 260 г/л, S 1,45, вносят 0,82 г гидроокиси алюминия (98%) и 90,33 г молотого силикагеля (содержание Al2O3 0,8 мас.), после чего, не прекращая перемешивания, приливают 85,58 г МЭА (99%-ного) и 12,97 г глицерина (98,5%-ного). Полученную реакционную смесь гомогенизируют перемешиванием в течение 0,5 ч при комнатной температуре (мольное отношение глицерина и воды равно 0,01), после чего загружают в автоклав и кристаллизуют в статических условиях при 150оС 150 ч. После окончания кристаллизации при этой температуре смесь подвергают охлаждению в автоклавe до 50оС со скоростью 7оС/ч. Продукт отфильтровывают, промывают дистиллированной водой до рН 7-8 и сушат при 120оС 10 ч. Получают цеолит типа ZSM-5.PRI me R. A reaction mixture is prepared with the following molar ratio of ingredients: Na 2 O 50 MEA 53 C 8 H 3 O Al 2 O 3 50 SiO 2 535 H 2 O, where MEA is monoethanolamine, for which 6.31 ml of aluminate solution is added to 254 ml of distilled water sodium (Na 2 O 272.8 g / l, Al 2 O 3 260 g / l, S 1.45, contribute 0.82 g of aluminum hydroxide (98%) and 90.33 g of ground silica gel (Al 2 O 3 content 0.8 wt.), After which 85.58 g of MEA (99%) and 12.97 g of glycerol (98.5%) were added without stopping stirring, and the resulting reaction mixture was homogenized by stirring for 0, 5 h at room temperature (molar ratio of glyc Erin and water equal to 0.01), and then charged into the autoclave and crystallized under static conditions at 150 C for 150 hours. After completion of crystallization at this temperature the mixture was cooled in avtoklave to 50 ° C at a rate of 7 C / hour. The product filtered off, washed with distilled water to a pH of 7-8 and dried at 120 ° C. for 10 hours. A zeolite of the type ZSM-5 was obtained.

Образцы полученных цеолитов подвергают рентгенофазовому анализу (ДРОН-3) с целью определения степени кристалличности, химанализу и определению адсорбционной емкости по парам н-гептана и бензола при Р/Рs 0,4.Samples of the obtained zeolites are subjected to x-ray phase analysis (DRON-3) in order to determine the degree of crystallinity, chemical analysis and determination of the adsorption capacity for pairs of n-heptane and benzene at P / P s 0.4.

Результаты остальных опытов и данные прототипа представлены в таблице. The results of the remaining experiments and the data of the prototype are presented in the table.

Таким образом, предложенный способ позволяет повысить степень кристалличности продукта. Thus, the proposed method allows to increase the degree of crystallinity of the product.

Claims (1)

СПОСОБ ПОЛУЧЕНИЯ ВЫСОКОКРЕМНЕЗЕМНОГО ЦЕОЛИТА ТИПА ZSM-5, включающий смешение источников кремния, алюминия, гидроокиси щелочного металла и воды, гидротермальную кристаллизацию смеси, последующее охлаждение смеси до 50oС со скоростью 5 10oС / ч, фильтрацию, промывку и сушку продукта, отличающийся тем, что, с целью повышения степени кристалличности продукта, на смешение дополнительно подают амин или диамин, или триамин, или тетрамин, или аминоспирт и глицерин, или этиленгликоль, или диэтиленгликоль, или метилэтилкетон, или этанол, или изопропанол, или изобутанол в количестве, обеспечивающем их молярное соотношение с водой, равное (0,005 0,051) 1 соответственно.METHOD FOR PRODUCING HIGH-SILICA ZEOLITE TYPE ZSM-5, including mixing sources of silicon, aluminum, alkali metal hydroxide and water, hydrothermal crystallization of the mixture, subsequent cooling of the mixture to 50 o C at a rate of 5 10 o C / h, filtration, washing and drying of the product, different in that, in order to increase the crystallinity of the product, an amine or diamine, or triamine, or tetramine, or amino alcohol and glycerin, or ethylene glycol, or diethylene glycol, or methyl ethyl ketone, or ethanol, or isopropane are additionally fed for mixing l, or isobutanol in an amount providing their molar ratio with water equal to (0.005 0.051) 1, respectively.
SU4366373 1988-01-20 1988-01-20 Method of preparing high-silicon zeolite type zsm-5 RU1610777C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU4366373 RU1610777C (en) 1988-01-20 1988-01-20 Method of preparing high-silicon zeolite type zsm-5

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SU4366373 RU1610777C (en) 1988-01-20 1988-01-20 Method of preparing high-silicon zeolite type zsm-5

Publications (1)

Publication Number Publication Date
RU1610777C true RU1610777C (en) 1995-06-27

Family

ID=30440878

Family Applications (1)

Application Number Title Priority Date Filing Date
SU4366373 RU1610777C (en) 1988-01-20 1988-01-20 Method of preparing high-silicon zeolite type zsm-5

Country Status (1)

Country Link
RU (1) RU1610777C (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EA000242B1 (en) * 1996-03-21 1999-02-25 Эниричерке С.П.А. Ers-10 zeolite and process for its preparation
CN100408181C (en) * 2005-08-15 2008-08-06 中国石油化工股份有限公司 Method for preparing catalyst of para xylene through form selected methylation of toluene

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Авторское свидетельство СССР N 1524395, кл. C 01B 33/28, 1987. *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EA000242B1 (en) * 1996-03-21 1999-02-25 Эниричерке С.П.А. Ers-10 zeolite and process for its preparation
CN100408181C (en) * 2005-08-15 2008-08-06 中国石油化工股份有限公司 Method for preparing catalyst of para xylene through form selected methylation of toluene

Similar Documents

Publication Publication Date Title
Millini et al. Synthesis and characterization of boron‐containing molecular sieves
US5194235A (en) Synthesis of SSZ-16 zeolite catalyst
US4404175A (en) Preparation of zeolites
KR102179936B1 (en) Post-treatment of a zeolitic material
US4478950A (en) Activity enhancement of high silica zeolites by thermal treatment with alkaline aluminate
CN103964465B (en) A kind of synthetic method of phosphorous ZSM-5 molecular sieve
RU1610777C (en) Method of preparing high-silicon zeolite type zsm-5
EP0086543B1 (en) Crystalline silicate catalysts with deactivated external surface, and process for its deactivation
EP0132049A1 (en) Process for separating a carboxylic acid of 1-8 carbon atoms from a mixture thereof with water and/or one or more other oxygenated aliphatic compounds
CN102897793B (en) Sodium-free synthesis method for ZSM-5 molecular sieve
JPH0154285B2 (en)
CN102897789B (en) Synthesis method for ZSM-5 molecular sieve
CN103964466B (en) 5 molecular sieves of a kind of ZSM and preparation method thereof
CN102897791B (en) Synthesis method for ZSM-5 molecular sieve
JPS5815024A (en) Manufacture of zeolite
EP0113473A1 (en) Novel zeolite catalyst and process for preparing same
CN102897790B (en) Synthesis method for ZSM-5 molecular sieve
EP0101254A2 (en) Process for separating ethanol from dilute aqueous solutions thereof
RU1799354C (en) Method for modified zeolite production
RU2156735C1 (en) Method of preparing high-silica zeolites
JPS59164617A (en) Super pure crystalline silica polyhedron and manufacture
RU2731469C1 (en) Method of producing zsm-12 flake zeolite with mtw structure
SU1472447A1 (en) Method of producing high-silica zeolite
RU2103226C1 (en) Method for producing high-silica zeolites
KR960011429B1 (en) Process for the preparation of zsm-5 and mordenite by gas transportation method