CN103787364A

CN103787364A - Method for preparing mordenite by using diatomite

Info

Publication number: CN103787364A
Application number: CN201410038385.0A
Authority: CN
Inventors: 胡涛; 吕楠; 孟长功; 张依福
Original assignee: Dalian University of Technology
Current assignee: Dalian University of Technology
Priority date: 2014-01-23
Filing date: 2014-01-23
Publication date: 2014-05-14

Abstract

The invention discloses a method for preparing mordenite by using diatomite and belongs to the field of production and preparation of inorganic functional materials. The method is characterized by comprising the following steps of: firstly determining the content of SiO2 and Al2O3 in a diatomite raw material, screening through a screen, and then drying in a drying box; uniformly mixing the dried diatomite raw material with deionized water and water glass, wherein the proportion of reaction raw materials in the formula is as follows: H2O/Na2O=8-11, Na2O/SiO2=0.05-0.30, SiO2/Al2O3=12-16; transferringthe material into a reaction kettle, and crystallizing at constant temperature; finally filtering, washing and drying the product to obtain the mordenite. According to the method disclosed by the invention, mordenite is prepared from the low-cost raw material diatomite; few diatomite pretreatment steps are carried out; and the energy source is saved through use of direct hydrothermal method synthesis. The preparation process has the advantages of simple process, easy operation and environmental friendliness.

Description

A kind of method of preparing mordenite with diatomite

Technical field

The invention belongs to the manufacture field of inorganic functional material, relate to a kind of with diatomite and industrial-grade sodium silicate be the method that raw material is prepared mordenite.

Background technology

3.2 hundred million tons of China's diatomite reserves, prospective reserves reaches more than 20 hundred million tons, accounts for 11.6% of world's total reserves.Diatomaceous main component comprises SiO ₂, Al ₂o ₃, Fe ₂o ₃, CaO, MgO and organic etc., wherein SiO ₂, Al ₂o ₃account for the overwhelming majority of content.Take diatomite as raw material, adopting hydrothermal synthesis method synthesis zeolite is a kind of important channel of diatomite deep exploitation.The method processing step of current existing synthesizing flokite is loaded down with trivial details, high with the synthetic cost of chemical reagent, the large and contaminate environment of Mother liquid.Therefore lack one take diatomite as raw material, mix with industrial reagent, adopt the method for hydrothermal synthesis method synthesizing flokite.

Summary of the invention

The technical problem to be solved in the present invention is to provide a kind of method of preparing mordenite with diatomite, and its technological process is simple, and energy consumption is low, can reduce the synthetic cost of mordenite by the method, increases economic benefit, protection of the environment.Prepare mordenite take diatomite as raw material, for mordenite synthetic provides a kind of cheap, abundant new raw material of originating.

Technical scheme of the present invention is:

Diatomite is sieved, dry.In stainless steel cauldron, add successively by a certain percentage water, water glass, diatomite, stir, sealing is placed in Constant Temp. Oven, crystallization for some time at a certain temperature, through suction filtration, washing, dry, can prepare mordenite.By feed change proportioning, crystallization temperature and crystallization time, can regulate the degree of crystallinity of product.

Kerosene shale ash raw material, formula rate and crystallization condition used when preparation are as follows:

Step 1: by after diatomite screening, after being dried, it is evenly mixed with deionized water, water glass, as reaction raw materials.When dry, can be chosen in 80～120 ℃ of condition baking ovens and be dried 12～24 hours.

Step 2: reaction raw materials mixes in reactor by following formula rate: H ₂o/Na ₂o=8～11, Na ₂o/SiO ₂=0.05～0.30, SiO ₂/ Al ₂o ₃=12～16, under normal temperature, stir 0.5～1h.

Step 3.: crystallization 15h～24h under the constant temperature of 150 ℃～180 ℃.

Step 4: obtain mordenite after product is filtered, washed to PH=7, is dried.

Effect of the present invention and benefit are can realize low cost raw material diatomite and industrial-grade sodium silicate and prepare mordenite molecular sieve pure phase.Diatomaceous pre-treatment is simple, there is no unnecessary thermal treatment and acid treatment, save energy.In preparation flow, do not use organic formwork agent, technique is simple, easy handling, and product is mordenite pure phase, reaction reproducibility is high.The present invention has significant advantage at aspects such as preparation cost, product performance, technical process, environmental friendliness and economic profits, and raw material sources are abundant, with low cost, and synthetic easy, equipment requirements is low, and product performance are high, possess suitability for industrialized production potentiality.

Embodiment

Below in conjunction with the detailed specific embodiments of the invention of technical scheme.

Embodiment 1

(1) mordenite is ground, cross 100 mesh sieves, in the baking oven of 90 ℃, be dried 24 hours.

Its main chemical constitution is as follows through XRF results of elemental analyses:

Chemical composition	SiO ₂	Al ₂O ₃	Fe ₂O ₃	K ₂O	TiO ₂	CaO	MgO	Na ₂O
									Per-cent %	79.5	10.5	5.8	1.3	0.9	0.6	0.5	0.3

The composition of the water glass that adopts is as follows:

Chemical composition	Na ₂O	SiO ₂	H ₂O
				Per-cent %	10.1	28	61.9

(2) H in molar ratio ₂o/Na ₂o=9.3 takes water glass and deionized water, in stainless steel cauldron, mixes, and then presses Na ₂o/SiO ₂=0.15 adds diatomite, stirs 0.5h and mixes.

(3) above-mentioned reaction mixture sealing is placed in 180 ℃ of Constant Temp. Ovens to crystallization 16h.

(4) take out reactor, carry out after cooling suction filtration, wash to PH=7, put into 100 ℃ of baking ovens dry, obtain mordenite crystal powder.

Embodiment 2

(1) diatomite is ground, cross 80 mesh sieves, in the baking oven of 100 ℃, be dried 12 hours.

(2) H in molar ratio ₂o/Na ₂o=10.9 weighing sodium hydroxide and deionized water mix in stainless steel cauldron, then press Na ₂o/SiO ₂=0.26 adds diatomite, stirs 1h and mixes.

(3) above-mentioned reaction mixture sealing is placed in 150 ℃ of Constant Temp. Ovens to crystallization 22h.

Claims

1. a method of preparing mordenite with diatomite, is characterized in that following steps:

Step 1: by dry after diatomite screening, then evenly mix with deionized water, water glass, as reaction raw materials;

Step 2: raw material mixes in reactor by following formula: H ₂o/Na ₂o=8～11, Na ₂o/SiO ₂=0.05～0.30, SiO ₂/ Al ₂o ₃=12～16, stirring at normal temperature 0.5～1h;

Step 3: crystallization 15h～24h under the constant temperature of 150 ℃～180 ℃;

Step 4: product is filtered, washed, obtain mordenite after being dried.

2. method according to claim 1, is characterized in that: after diatomite is crossed to the screening of 40-100 mesh sieve, be dried.

3. method according to claim 1 and 2, is characterized in that: when dry, be chosen in 80～110 ℃ of baking ovens and be dried 12～24 hours.