CN105854412B - Compound filtering material suitable for purifying ionic liquid and filtering method - Google Patents

Compound filtering material suitable for purifying ionic liquid and filtering method Download PDF

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Publication number
CN105854412B
CN105854412B CN201610231156.XA CN201610231156A CN105854412B CN 105854412 B CN105854412 B CN 105854412B CN 201610231156 A CN201610231156 A CN 201610231156A CN 105854412 B CN105854412 B CN 105854412B
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ionic liquid
diatomite
parts
mesh
filtering
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CN105854412A (en
Inventor
李瑞丰
张军
张晓煜
余坚
邱金江
武进
李军波
张金明
张东光
崔增亮
王德坤
王新
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Shandong Zhongke Heng Lian Biological Base Material Co Ltd
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Shandong Zhongke Heng Lian Biological Base Material Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/02Loose filtering material, e.g. loose fibres
    • B01D39/06Inorganic material, e.g. asbestos fibres, glass beads or fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D37/00Processes of filtration
    • B01D37/02Precoating the filter medium; Addition of filter aids to the liquid being filtered

Abstract

The invention discloses a compound filter material suitable for purifying ionic liquid and a filtering method thereof. The diatomite with different meshes is selected from at least two of the following meshes: 100 meshes, 200 meshes, 600 meshes and 1000 meshes. 1) Uniformly mixing diatomite with different granularities according to a set mass ratio to obtain a compound filter material; 2) preparing a diatomite solution from the compound filter material by using ionic liquid to be filtered, and forming a diatomite precoat layer on the filter plate; 3) the ionic liquid to be filtered was filtered through a celite precoat. The compound filter material can filter the ionic liquid with the concentration of more than 95 wt%, and the filtering speed reaches 1-3 tons/h, thereby obviously improving the filtering speed of the ionic liquid with high concentration and high viscosity. The filtered ionic liquid is clear and transparent, and the turbidity is 0.5-5 degrees, so that the filtering precision of the filtered ionic liquid is greatly improved.

Description

Compound filtering material suitable for purifying ionic liquid and filtering method
Technical Field
The invention relates to a compound filtering material suitable for purifying ionic liquid and a filtering method, and belongs to the field of ionic liquid filtering.
Background
Diatomite is a siliceous rock with SiO as the main chemical component2And the color of the product can be white, light yellow or light gray due to different impurity types and contents. The diatomite has a special porous structure and relatively high porosity, so that the diatomite has special physical properties of strong adsorbability, light weight, sound insulation, heat resistance and the like. It is used as heat insulating material, filtering material, stuffing, grinding material, water glass material, decolorizing agent, diatomite filter aid, catalyst carrier, etc.
At present, many reports of filtering by using diatomite exist at home and abroad, such as filtering beer, fruit juice beverage, illegal cooking oil and the like, but materials with high viscosity are filtered by using the diatomite, and particularly ionic liquid with high filtering viscosity is not reported.
The ionic liquid is an organic salt composed of organic cations and organic or inorganic anions, has the advantages of nonvolatility, high thermal stability and chemical stability, good solubility, adjustable performance, easy separation, easy recovery and recycling and the like, is known as a green solvent with excellent performance, and has important application prospects in the fields of chemical synthesis, extraction separation, electrochemistry, material preparation, environmental engineering, energy chemistry and the like. In recent years, the application of ionic liquid in the processing of cellulose has attracted wide attention at home and abroad. In the recovery of the ionic liquid, the separation from other solvents can be performed by distillation, and the separation from solids is often performed by filtration. The diatomite has good filtering effect when filtering liquid materials with low viscosity. However, after the recovered ionic liquid is concentrated, the viscosity is obviously improved along with the increase of the concentration, particularly after the concentration reaches 95 wt%, the ionic liquid is difficult to be efficiently filtered by common diatomite, the filtering speed is very slow, the filtering efficiency is influenced, the filtering precision is insufficient, and great difficulty is caused to the actual production.
In the 2015100076503 patent, diatomite is used as a filter medium to recover and filter the ionic liquid, the diatomite with the granularity of 200-600 meshes is prepared into a diatomite solution by the ionic liquid, a diatomite layer is formed by a filter, and the high-viscosity ionic liquid is filtered by the filter forming the diatomite layer, so that the filtering speed of the ionic liquid is improved. However, the method is only applicable to the ionic liquid with the concentration of less than 90 wt%, and the turbidity of the filtered ionic liquid is 20-130 degrees and is still high. At present, no effective filtration method exists for ionic liquid with the concentration of more than 90 wt%.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a compound filter material and a filter method suitable for purifying ionic liquid, the filter material can filter the ionic liquid with the concentration of more than 90 wt%, the filter speed is high, the turbidity of the filtered ionic liquid is low, and the rapid and high-precision filtration of the ionic liquid is realized.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a compound filter material suitable for purifying ionic liquid is prepared by mixing diatomite with different meshes according to a set mass ratio; the diatomite with different meshes is selected from at least two of the following meshes: 100 meshes, 200 meshes, 600 meshes and 1000 meshes.
Preferably, the diatomite of 100 meshes, 200 meshes, 600 meshes and 1000 meshes is prepared by mixing the following components in percentage by mass: 15-70: 15-70: 5-80: 5-60.
Still further preferably, the compound filter material consists of the following components in parts by weight:
50-80 parts of 100-mesh diatomite, 10-20 parts of 200-mesh diatomite and 5-20 parts of 600-mesh diatomite;
or 10-40 parts of 100-mesh diatomite, 10-70 parts of 200-mesh diatomite and 40-60 parts of 1000-mesh diatomite;
or 10-30 parts of 100-mesh diatomite, 50-80 parts of 600-mesh diatomite and 5-20 parts of 1000-mesh diatomite;
or 10-30 parts of 200-mesh diatomite, 50-80 parts of 600-mesh diatomite and 10-30 parts of 1000-mesh diatomite.
The compound filter material is applied to the ionic liquid with the filtering concentration of more than 90 wt%.
The method for filtering the ionic liquid by using the compound filter material comprises the following steps:
(1) uniformly mixing diatomite with different granularities according to a set mass ratio to obtain a compound filter material;
(2) preparing a diatomite solution from the compound filter material by using ionic liquid to be filtered, and forming a diatomite precoat layer on the filter plate;
(3) the ionic liquid to be filtered was filtered through a celite precoat.
Preferably, in the step (2), the concentration of the diatomite solution is 2-5 wt%.
Preferably, the concentration of the ionic liquid is 90 to 97 wt%.
Further preferably, the ionic liquid has a concentration of 95 wt% and a viscosity of 38 mpa.s.
Preferably, the dosage of the diatomite in the diatomite precoat is 1.2-6.7kg/m2
Preferably, in the step (3), the filtration speed of the ionic liquid is 1-3 t/h.
Preferably, in the step (3), the turbidity of the filtered ionic liquid is less than 5 degrees.
The application of the method in filtering ionic liquid with the concentration of more than 90 wt%. The ionic liquid comprises: N-ethyl-N, -methylimidazole chloride ionic liquid, N-propyl-N, -methylimidazole chloride ionic liquid, N-butyl-N, -methylimidazole chloride ionic liquid, N-allyl-N, -methylimidazole chloride ionic liquid, N-methylallyl-N, -methylimidazole chloride ionic liquid, N-ethyl-N, -methylimidazole acetate ionic liquid, N-propyl-N, -methylimidazole acetate ionic liquid, N-butyl-N, -methylimidazole acetate ionic liquid, N-allyl-N, -methylimidazole acetate ionic liquid or N-methylallyl-N, -methylimidazole acetate ionic liquid.
When a tester begins to perform an experiment, diatomite with a single mesh number is adopted for filtering, and after filtering, the diatomite with different mesh numbers has different filtering effects and filtering speeds, and the diatomite with different mesh numbers is suitable for ionic liquids with different concentrations; for the ionic liquid with the concentration of more than 95 wt%, the diatomite with single mesh number has the disadvantages of slow filtration speed or poor filtration effect when in use: the low mesh diatomite has poor filtering effect, and the high mesh diatomite has low filtering speed. Therefore, the test personnel cooperate with the diatomite with different meshes to test the filtering effect, optimize the combination, and integrate the advantages of the diatomite with high and low meshes so as to meet the filtering requirement of the high-concentration ionic liquid.
The beneficial technical effects of the invention are as follows:
1. the compound filter material can filter the ionic liquid with the concentration of more than 90 wt%, and the filtering speed reaches 1-3 tons/h, thereby obviously improving the filtering speed of the ionic liquid with high concentration and high viscosity.
2. The ionic liquid filtered by the compound filter material is clear and transparent, the turbidity is less than 5 degrees, and the filtering precision of the ionic liquid is greatly improved.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 200 meshes and 600 meshes is added according to the proportion of 15%: 80%: 5 percent of the diatomite is uniformly mixed together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.5kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered in advance, then the ionic liquid with the concentration of 95 wt% and the viscosity of 38mpa.s is smoothly filtered through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 0.5 degrees, and the filtering speed is 2 tons/h.
Example 2
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 200 meshes and 600 meshes is added according to the proportion of 70%: 15%: uniformly mixing 15% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.2kg/m2In an amount such that a pre-coating of diatomaceous earth is formed using the ionic liquid to be filteredAnd then, smoothly filtering the ionic liquid with the concentration of 97 wt% and the viscosity of 40mpa.s through a precoat layer, wherein the filtered ionic liquid is clear and transparent, the turbidity is 4 degrees, and the filtering speed is 3 tons/h.
Example 3
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 200 meshes and 1000 meshes is mixed according to the proportion of 20%: 20%: uniformly mixing 60% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.4kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered in advance, then the ionic liquid with the concentration of 93 wt% and the viscosity of 36mpa.s is smoothly filtered through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 0.5 degrees, and the filtering speed is 0.5 ton/h.
Example 4
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 200 meshes and 1000 meshes is mixed according to the proportion of 15%: 70%: uniformly mixing 15% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.5kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered in advance, then the ionic liquid with the concentration of 97 wt% and the viscosity of 40mpa.s is smoothly filtered through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 1 degree, and the filtering speed is 1.5 tons/h.
Example 5
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 600 meshes and 1000 meshes is mixed according to the proportion of 20%: 60%: uniformly mixing 20% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.6kg/m2The amount of (A) is determined by pre-forming a pre-coating of diatomaceous earth with the ionic liquid to be filtered, and then filtering the ionic liquid with a concentration of 92 wt% and a viscosity of 36mpa.s smoothly through the pre-coating, the filtered ionic liquid being clear and transparent and having a turbidity of3.5 degrees, and the filtering speed is 1 ton/h.
Example 6
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 600 meshes and 1000 meshes is mixed according to the proportion of 15%: 80%: 5 percent of the diatomite is uniformly mixed together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.5kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered in advance, then the ionic liquid with the concentration of 90 wt% and the viscosity of 35mpa.s is filtered by smoothly passing through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 2 degrees, and the filtering speed is 1.5 tons/h.
Example 7
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 200 meshes, 600 meshes and 1000 meshes is added according to the proportion of 15%: 70%: uniformly mixing 15% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.7kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered in advance, then the ionic liquid with the concentration of 95 wt% and the viscosity of 38mpa.s is smoothly filtered through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 2.5 degrees, and the filtering speed is 1.5 tons/h.
Example 8
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 200 meshes, 600 meshes and 1000 meshes is added according to the proportion of 20%: 60%: uniformly mixing 20% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 0.8kg/m2The diatomite precoating is formed in advance by using the ionic liquid to be filtered, then the ionic liquid with the concentration of 95 wt% and the viscosity of 38mpa.s is smoothly filtered through the precoating, the filtered ionic liquid is clear and bright, the turbidity is 2 degrees, and the filtering speed is 2 tons/h.
Example 9
A compound filter material suitable for purifying ionic liquid is implemented as follows:
200-mesh and 600-mesh diatomite are mixed according to the weight ratio of 40%: uniformly mixing 60% of the components together in a mass ratio to prepare compound diatomite; the diatomite is adopted according to the proportion of 1.2kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered, then the ionic liquid with the concentration of 95 wt% and the viscosity of 38mpa.s is smoothly filtered through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 4 degrees, and the filtering speed is 1.8 tons/h.
Example 10
A compound filter material suitable for purifying ionic liquid is implemented as follows:
diatomite of 100 meshes, 200 meshes, 600 meshes and 1000 meshes is mixed according to the weight ratio of 20: 60: 20: 30, and preparing the compound diatomite; the diatomite is adopted according to the proportion of 1.5kg/m2The diatomite precoat is formed by using the ionic liquid to be filtered, then the ionic liquid with the concentration of 95 wt% and the viscosity of 38mpa.s is smoothly filtered through the precoat, the filtered ionic liquid is clear and bright, the turbidity is 4 degrees, and the filtering speed is 3 tons/h.
By adopting the process formula, the high-viscosity ionic liquid can be filtered, the filtering speed is high, the filtering precision is high, the filtered ionic liquid has fewer impurities and is clear and bright, and the high-viscosity ionic liquid is a novel compound formula for filtering the high-viscosity ionic liquid.
Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (8)

1. The application of the compound filter material in filtering ionic liquid with the concentration of more than 90 wt% is characterized in that:
the compound filter material comprises the following components in parts by weight:
50-80 parts of 100-mesh diatomite, 10-20 parts of 200-mesh diatomite and 5-20 parts of 600-mesh diatomite;
or 10-40 parts of 100-mesh diatomite, 10-70 parts of 200-mesh diatomite and 40-60 parts of 1000-mesh diatomite;
or 10-30 parts of 100-mesh diatomite, 50-80 parts of 600-mesh diatomite and 5-20 parts of 1000-mesh diatomite;
or 10-30 parts of 200-mesh diatomite, 50-80 parts of 600-mesh diatomite and 10-30 parts of 1000-mesh diatomite.
2. A method of filtering ionic liquids using a compounded filter material, comprising: the method comprises the following steps:
1) uniformly mixing diatomite with different granularities according to a set mass ratio to obtain a compound filter material;
2) preparing a diatomite solution from the compound filter material by using ionic liquid to be filtered, and forming a diatomite precoat layer on the filter plate;
3) filtering the ionic liquid to be filtered through a diatomite precoat;
the compound filter material comprises the following components in parts by weight:
50-80 parts of 100-mesh diatomite, 10-20 parts of 200-mesh diatomite and 5-20 parts of 600-mesh diatomite;
or 10-40 parts of 100-mesh diatomite, 10-70 parts of 200-mesh diatomite and 40-60 parts of 1000-mesh diatomite;
or 10-30 parts of 100-mesh diatomite, 50-80 parts of 600-mesh diatomite and 5-20 parts of 1000-mesh diatomite;
or 10-30 parts of 200-mesh diatomite, 50-80 parts of 600-mesh diatomite and 10-30 parts of 1000-mesh diatomite.
3. The method of claim 2, wherein: in the step 2), the concentration of the diatomite solution is 2-5 wt%.
4. The method of claim 3, wherein: the concentration of the ionic liquid is 90-97 wt%.
5. The method of claim 4, wherein: the ionic liquid has a concentration of 95 wt% and a viscosity of 38 mpa.s.
6. The method of claim 2, wherein: in the diatomite precoating layer, the dosage of the diatomite is 1.2-6.7kg/m2
Or in the step 3), the filtering speed of the ionic liquid is 1-3t/h, and the turbidity of the filtered ionic liquid is less than 5 degrees.
7. Use of the method of any one of claims 2 to 6 for filtering ionic liquids having a concentration of greater than 90% by weight.
8. Use according to claim 7, characterized in that: the ionic liquid is N-ethyl-N, -methylimidazole chloride ionic liquid, N-propyl-N, -methylimidazole chloride ionic liquid, N-butyl-N, -methylimidazole chloride ionic liquid, N-allyl-N, -methylimidazole chloride ionic liquid, N-methylallyl-N, -methylimidazole chloride ionic liquid, N-ethyl-N, -methylimidazole acetate ionic liquid, N-propyl-N, -methylimidazole acetate ionic liquid, N-butyl-N, -methylimidazole acetate ionic liquid, N-allyl-N, -methylimidazole acetate ionic liquid or N-methylallyl-N, -methylimidazole acetate ionic liquid.
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