阅读说明：本技术 一种用于油水分离的超疏水滤纸的制备方法 (Preparation method of super-hydrophobic filter paper for oil-water separation ) 是由 马静蕊 李晓 郭探 云山 陈静 于 2021-08-27 设计创作，主要内容包括：本发明公开了一种用于油水分离的超疏水滤纸的制备方法,包括以下步骤：(1)将凹凸棒石黏土与纸浆混合均匀得到混合浆料,将混合浆料进行抽滤后,压平晾干得到含凹凸棒石黏土的滤纸；(2)将装有烷基三烷氧基硅烷的敞口容器与步骤(1)制得的含凹凸棒石黏土的滤纸一同放入带冷凝装置的密闭反应器中,将密闭反应器进行加热促进烷基三烷氧基硅烷挥发产生蒸汽对含凹凸棒石黏土的滤纸进行疏水改性,得到超疏水滤纸,改性过程中产生的有机蒸汽通过冷凝装置回收。本发明的制备方法简单环保,不使用有机溶剂,无废气废液产生,易于规模化制备超疏水滤纸。制得的超疏水滤纸用于油水分离的时候,可以重复进行油水分离500次以上。(The invention discloses a preparation method of super-hydrophobic filter paper for oil-water separation, which comprises the following steps: (1) uniformly mixing attapulgite clay and paper pulp to obtain mixed slurry, performing suction filtration on the mixed slurry, and flattening and airing to obtain filter paper containing the attapulgite clay; (2) putting the open container filled with the alkyl trialkoxysilane and the attapulgite clay-containing filter paper prepared in the step (1) into a closed reactor with a condensing device, heating the closed reactor to promote the volatilization of the alkyl trialkoxysilane to generate steam to perform hydrophobic modification on the attapulgite clay-containing filter paper to obtain super-hydrophobic filter paper, and recovering organic steam generated in the modification process through the condensing device. The preparation method is simple and environment-friendly, does not use organic solvent, does not generate waste gas and waste liquid, and is easy for large-scale preparation of the super-hydrophobic filter paper. When the prepared super-hydrophobic filter paper is used for oil-water separation, the oil-water separation can be repeatedly carried out for more than 500 times.)

1. A preparation method of super-hydrophobic filter paper for oil-water separation is characterized by comprising the following steps:

(1) uniformly mixing attapulgite clay and paper pulp to obtain mixed slurry, performing suction filtration on the mixed slurry, and flattening and airing to obtain filter paper containing the attapulgite clay;

(2) putting the open container filled with the alkyl trialkoxysilane and the attapulgite clay-containing filter paper prepared in the step (1) into a closed reactor with a condensing device, heating the closed reactor to promote the volatilization of the alkyl trialkoxysilane to generate steam to perform hydrophobic modification on the attapulgite clay-containing filter paper to obtain super-hydrophobic filter paper, and recovering organic steam generated in the modification process through the condensing device.

2. The method for preparing the superhydrophobic filter paper for oil-water separation according to claim 1, wherein the method comprises the following steps: the alkyltrialkoxysilane in the step (2) is one or a mixture of more than two of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, octadecyltrimethoxysilane, octadecyltriethoxysilane, vinyltriethoxysilane or vinyltrimethoxysilane.

3. The method for preparing the superhydrophobic filter paper for oil-water separation according to claim 1, wherein the method comprises the following steps: the heating temperature in the step (2) is 50-100 ℃.

4. The method for preparing the superhydrophobic filter paper for oil-water separation according to claim 1, wherein the method comprises the following steps: the modification time in the step (2) is 0.5-4 h.

5. The method for preparing the superhydrophobic filter paper for oil-water separation according to claim 1, wherein the method comprises the following steps: the attapulgite clay-containing filter paper prepared in the step (1) contains 1-5 wt% of attapulgite clay.

6. The application of the super-hydrophobic filter paper prepared by the method of any one of claims 1 to 5 in the field of oil-water separation.

Technical Field

The invention belongs to the field of preparation of super-hydrophobic materials, relates to preparation of super-hydrophobic filter paper, and particularly relates to a preparation method of super-hydrophobic filter paper for oil-water separation.

Background

Worldwide, petroleum leakage events are frequent, and a large amount of oil-water mixed liquid is generated in the industries of crude oil exploitation, mechanical processing, biochemical engineering and the like, so that the problem of oil-water separation is faced. The existing separation methods such as gravity separation, ultrasonic separation, centrifugal separation and the like have long separation time, large equipment size and secondary pollution in the treatment process. Therefore, the development of a novel efficient green filter material is urgently needed. The paper has the characteristics of low production cost, biodegradability, recyclability, good mechanical property and the like, and has great application potential in the field of oil-water separation and filtration.

In order to meet the requirements for oil-water separation, it is necessary to subject paper to a hydrophobization treatment. Chinese patent publication No. CN 111549568A discloses a preparation method of super-hydrophobic paper, which comprises the steps of mixing octadecylamine emulsion with paper pulp, adding tannic acid and aluminum chloride for reaction to form microcapsule modified paper pulp, and then flattening and drying to obtain the super-hydrophobic paper. Chinese patent publication No. CN 107401086a discloses a method for preparing super-hydrophobic paper, which comprises processes of primary spraying, baking, secondary spraying and the like, and the preparation is complicated, and there is pollution caused by solvent volatilization. Chinese patent publication No. CN 103653744A discloses a super-hydrophobic paper and a preparation method thereof, the preparation method is to modify the paper by hydroxylation, then increase the surface roughness of the paper by plasma etching, and finally treat the paper by a fluorine-containing reagent. The method needs expensive plasma etching equipment and has high production cost. Chinese patent publication No. CN 102808357a discloses super-hydrophobic paper and a preparation method thereof, wherein a modified nano-silica coating is first constructed on the surface of the paper, but the method requires the use of an organic solvent. Therefore, the development of an environment-friendly, simple and efficient preparation method of the super-hydrophobic paper is still needed, and the method is applied to the field of oil-water separation.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a preparation method of super-hydrophobic filter paper for oil-water separation.

The invention is realized by the following technical scheme:

a preparation method of super-hydrophobic filter paper for oil-water separation comprises the following steps:

(1) uniformly mixing attapulgite clay and paper pulp to obtain mixed slurry, performing suction filtration on the mixed slurry, and flattening and airing to obtain filter paper containing the attapulgite clay;

(2) putting the open container filled with the alkyl trialkoxysilane and the attapulgite clay-containing filter paper prepared in the step (1) into a closed reactor with a condensing device, heating the closed reactor to promote the volatilization of the alkyl trialkoxysilane to generate steam to perform hydrophobic modification on the attapulgite clay-containing filter paper to obtain super-hydrophobic filter paper, and recovering organic steam generated in the modification process through the condensing device.

The invention further improves the scheme as follows:

the alkyltrialkoxysilane in the step (2) is one or a mixture of more than two of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, octadecyltrimethoxysilane, octadecyltriethoxysilane, vinyltriethoxysilane or vinyltrimethoxysilane.

Further, the heating temperature in the step (2) is 50-100 ℃.

Further, the modification time in the step (2) is 0.5-4 h.

Further, the attapulgite clay-containing filter paper prepared in the step (1) contains 1-5 wt% of attapulgite clay.

The invention further improves the scheme as follows:

the super-hydrophobic filter paper prepared by the method is applied to the field of oil-water separation.

The invention has the beneficial effects that:

according to the invention, attapulgite is introduced into the filter paper, then rich active hydroxyl groups on the surface of the attapulgite directly react with the organosilane modifier to obtain the filter paper with super-hydrophobic property, and the hydrophobic groups are combined with the filter paper by chemical bonds, so that the filter paper is good in stability.

Due to the super-hydrophobic characteristic, the super-hydrophobic filter paper can enable oil to pass through and prevent water from passing through, so that oil-water separation is realized, and the prepared filter paper has good stability and can be repeatedly used for oil-water separation for more than 500 times.

The invention directly adopts the gas phase method for modification, avoids the need of a large amount of organic solvent in the traditional liquid phase method for modification, and recovers the organic steam generated in the modification process in a condensation mode without any waste gas emission.

The modification process disclosed by the invention does not need any complex modification equipment, is simple and environment-friendly, and is easy for large-scale preparation of the super-hydrophobic filter paper.

Drawings

FIG. 1 shows the formation of water droplets on the superhydrophobic filter paper prepared in example 1.

FIG. 2 is a contact angle of water on the superhydrophobic filter paper prepared in example 2, the contact angle being 158 °.

Detailed Description

Example 1

(1) Uniformly mixing attapulgite clay and paper pulp under high-speed stirring to obtain mixed slurry, performing suction filtration on the mixed slurry, flattening and drying to obtain the filter paper containing the attapulgite clay. Wherein the content of attapulgite clay in the filter paper is 1%.

(2) Pouring the methyltrimethoxysilane into an open container and putting the methyltrimethoxysilane and the filter paper prepared in the step (1) into a closed oven with a condensing device. And heating the oven to 50 ℃ for hydrophobic modification for 4h, recovering organic steam generated in the modification process by using a super-condensing device, and finally opening the oven to obtain the super-hydrophobic filter paper.

The contact angle of the prepared super-hydrophobic filter paper to water is 152 degrees, and oil-water separation can be repeatedly carried out for 550 times.

Example 2

(1) Uniformly mixing attapulgite clay and paper pulp under high-speed stirring to obtain mixed slurry, performing suction filtration on the mixed slurry, flattening and drying to obtain the filter paper containing the attapulgite clay. Wherein the content of attapulgite clay in the filter paper is 2%.

(2) Pouring the methyltriethoxysilane into an open container and putting the methyltriethoxysilane and the filter paper prepared in the step (1) into a closed oven with a condensing device. And heating the oven to 60 ℃ for hydrophobic modification for 3h, recovering organic steam generated in the modification process by using a super-condensing device, and finally opening the oven to obtain the super-hydrophobic filter paper.

The contact angle of the prepared super-hydrophobic filter paper to water is 158 degrees, and oil-water separation can be repeatedly carried out for 600 times.

Example 3

(1) Uniformly mixing attapulgite clay and paper pulp under high-speed stirring to obtain mixed slurry, performing suction filtration on the mixed slurry, flattening and drying to obtain the filter paper containing the attapulgite clay. Wherein the content of attapulgite clay in the filter paper is 5%.

(2) Pouring the vinyltriethoxysilane into an open container and putting the container and the filter paper prepared in the step (1) into a closed oven with a condensing device. And heating the oven to 100 ℃ for hydrophobic modification for 0.5h, recovering organic steam generated in the modification process by using a super-condensing device, and finally opening the oven to obtain the super-hydrophobic filter paper.

The contact angle of the prepared super-hydrophobic filter paper to water is 168 degrees, and oil-water separation can be repeatedly carried out for 1000 times.

Example 4

(1) Uniformly mixing attapulgite clay and paper pulp under high-speed stirring to obtain mixed slurry, performing suction filtration on the mixed slurry, flattening and drying to obtain the filter paper containing the attapulgite clay. Wherein the content of attapulgite clay in the filter paper is 4%.

(2) Pouring the propyltriethoxysilane into an open container and putting the propyltriethoxysilane and the filter paper prepared in the step (1) into a closed oven with a condensing device. And heating the oven to 80 ℃ for hydrophobic modification for 2h, recovering organic steam generated in the modification process by using a super-condensing device, and finally opening the oven to obtain the super-hydrophobic filter paper.

The contact angle of the prepared super-hydrophobic filter paper to water is 161 degrees, and oil-water separation can be repeatedly carried out for 850 times.

Example 4

(1) Uniformly mixing attapulgite clay and paper pulp under high-speed stirring to obtain mixed slurry, performing suction filtration on the mixed slurry, flattening and drying to obtain the filter paper containing the attapulgite clay. Wherein the content of attapulgite clay in the filter paper is 4%.

(2) Pouring the propyltriethoxysilane into an open container and putting the propyltriethoxysilane and the filter paper prepared in the step (1) into a closed oven with a condensing device. And heating the oven to 80 ℃ for hydrophobic modification for 2h, recovering organic steam generated in the modification process by using a super-condensing device, and finally opening the oven to obtain the super-hydrophobic filter paper.

The contact angle of the prepared super-hydrophobic filter paper to water is 161 degrees, and oil-water separation can be repeatedly carried out for 850 times.

Example 5

(1) Uniformly mixing attapulgite clay and paper pulp under high-speed stirring to obtain mixed slurry, performing suction filtration on the mixed slurry, flattening and drying to obtain the filter paper containing the attapulgite clay. Wherein the content of attapulgite clay in the filter paper is 3%.

(2) Pouring the octadecyl triethoxy silane into an open container and putting the octadecyl triethoxy silane and the filter paper prepared in the step (1) into a closed oven with a condensing device. And heating the oven to 90 ℃ for hydrophobic modification for 2h, recovering organic steam generated in the modification process by using a super-condensing device, and finally opening the oven to obtain the super-hydrophobic filter paper.

The contact angle of the prepared super-hydrophobic filter paper to water is 172 degrees, and the oil-water separation can be repeatedly carried out for 900 times.