阅读说明：本技术 甲醛吸附材料的制备方法 (Preparation method of formaldehyde adsorption material ) 是由 佘丽丽 杨志华 赵杨 郝浩 郑军妹 郭国良 于 2021-07-19 设计创作，主要内容包括：一种吸甲醛材料的制备方法,其特征在于包括如下步骤①将硅胶粉末放置在等离子体反应室中处理,处理后取出；②将份聚乙烯亚胺溶解在去离子水中并分散均匀,加入胺源并分散均匀；形成混合液；③在混合液中添加等离子体处理后的硅胶粉末,浸渍分散后经过过滤,取有效浸渍后的硅胶粉末并烘干,得到具有吸附甲醛功能的硅胶粉末；④将步骤③中获得的硅胶粉末与羧甲基纤维素和水混合,造粒、烘干,获得硅胶颗粒。使用等离子体处理后硅胶颗粒的亲水性能增强,在溶液浸渍过程中能负载更多乙烯脲。同时由于表面电子的存在,使胺源负载时可均匀分布在硅胶孔道内部和表面,提高材料的甲醛吸附性能。(A preparation method of formaldehyde absorbing material is characterized by comprising the following steps of firstly, placing silica gel powder in a plasma reaction chamber for treatment, and taking out the treated silica gel powder; dissolving part of polyethyleneimine in deionized water and uniformly dispersing, and adding an amine source and uniformly dispersing; forming a mixed solution; thirdly, adding the silica gel powder after plasma treatment into the mixed liquid, filtering after dipping and dispersing, taking the silica gel powder after effective dipping and drying to obtain the silica gel powder with the function of adsorbing formaldehyde; and fourthly, mixing the silica gel powder obtained in the third step with carboxymethyl cellulose and water, granulating and drying to obtain silica gel particles. The hydrophilic performance of the silica gel particles is enhanced after the plasma treatment, and more ethylene urea can be loaded in the solution impregnation process. Meanwhile, due to the existence of surface electrons, the amine source can be uniformly distributed inside and on the surface of the silica gel pore channel when being loaded, so that the formaldehyde adsorption performance of the material is improved.)

1. The preparation method of the formaldehyde absorbing material is characterized by comprising the following steps

Firstly, placing silica gel powder in a plasma reaction chamber for treatment, and taking out the treated silica gel powder;

dissolving part of polyethyleneimine in deionized water and uniformly dispersing, and adding an amine source and uniformly dispersing; forming a mixed solution;

thirdly, adding the silica gel powder after plasma treatment into the mixed liquid, filtering after dipping and dispersing, taking the silica gel powder after effective dipping and drying to obtain the silica gel powder with the function of adsorbing formaldehyde;

mixing the silica gel powder obtained in the step (III) with carboxymethyl cellulose and water, granulating and drying to obtain silica gel particles;

the weight ratio of the silica gel powder to the amine source meets the following requirements:

15-40 parts of silica gel powder;

5-15 parts of an amine source;

in the step IV, the weight ratio of the silica gel powder to the carboxymethyl cellulose meets the following requirements:

10-30 parts of silica gel powder;

5-10 parts of carboxymethyl cellulose.

2. The method of claim 1, wherein the amine source is at least one of ethylene urea, ammonium sulfate, or alanine.

3. The production method according to claim 1, wherein the plasma treatment conditions in step (i) are as follows:

treating with 100W low-temperature plasma under normal temperature and pressure oxygen flow for 10-30 min

4. The preparation method according to claim 1, wherein the dipping time in the step (c) is 1-6 hours

5. The method according to claim 1, wherein the drying conditions in step (c) are as follows: drying in microwave drying equipment, wherein the drying power is set to be 500-3000W, and the drying time is 0.5-2 h.

6. The method according to claim 1, wherein the drying conditions in the step (iv) are as follows: and drying for 10-50 min under the condition of hot air drying.

Technical Field

The invention relates to a formaldehyde adsorption material, and belongs to the technical field of air purification.

Background

The existing formaldehyde adsorption material mainly comprises active carbon, silica gel, molecular sieve and zeolite, and is mainly used for physical adsorption or chemical adsorption by loading active ingredients capable of reacting with formaldehyde in the materials. However, most of the materials are mesoporous or microporous materials, long time is needed for loading substances, the loading degree of chemical substances is limited, and the preparation time and the formaldehyde adsorption effect of the materials are influenced to a certain extent.

Disclosure of Invention

The invention aims to solve the technical problem of providing a preparation method of a formaldehyde adsorption material with short preparation time and good formaldehyde adsorption effect aiming at the technical current situation.

The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the formaldehyde absorbing material is characterized by comprising the following steps

Firstly, placing silica gel powder in a plasma reaction chamber for treatment, and taking out the treated silica gel powder;

dissolving part of polyethyleneimine in deionized water and uniformly dispersing, and adding an amine source and uniformly dispersing; forming a mixed solution;

thirdly, adding the silica gel powder after plasma treatment into the mixed liquid, filtering after dipping and dispersing, taking the silica gel powder after effective dipping and drying to obtain the silica gel powder with the function of adsorbing formaldehyde;

mixing the silica gel powder obtained in the step (III) with carboxymethyl cellulose and water, granulating and drying to obtain silica gel particles;

the weight ratio of the silica gel powder to the amine source meets the following requirements:

15-40 parts of silica gel powder;

5-15 parts of an amine source;

in the step IV, the weight ratio of the silica gel powder to the carboxymethyl cellulose meets the following requirements:

10-30 parts of silica gel powder;

5-10 parts of carboxymethyl cellulose.

Preferably, the amine source is at least one of ethylene urea, ammonium sulfate or alanine.

Preferably, the plasma treatment conditions in step (r) are as follows:

treating with 100W low-temperature plasma under normal temperature and pressure oxygen flow for 10-30 min

Preferably, the dipping time in the step III is 1-6 hours

Preferably, the drying conditions in the third step are as follows: drying in microwave drying equipment, wherein the drying power is set to be 500-3000W, and the drying time is 0.5-2 h.

Preferably, the drying conditions in the step (iv) are as follows: and drying for 10-50 min under the condition of hot air drying.

Compared with the prior art, the invention has the advantages that:

the plasma treatment can generate free radicals (H) on the surface of the silica gel powder₂O+SiO₂→SiO₂-OH+SiO₂-O radical + SiO₂-OH radicals). The surface of the silica gel powder can be roughened due to the strong oxidizing property of the free radicals, so that the specific surface area of the silica gel powder is increased.

The plasma treatment can enhance the cohesiveness of the surface of the silica gel powder, and is convenient for preparing silica gel particles. The strength and the wear resistance of the prepared silica gel particles are enhanced.

The hydrophilic performance of the silica gel particles is enhanced after the plasma treatment, and more ethylene urea can be loaded in the solution impregnation process. Meanwhile, due to the existence of surface electrons, the amine source can be uniformly distributed inside and on the surface of the silica gel pore channel when being loaded, so that the formaldehyde adsorption performance of the material is improved.

The plasma treatment enables the amine source to grow on the surface of the silica gel rapidly, the chemical substance loading time can be reduced, the common mechanical loading needs to be carried out for more than 12 hours, and the loading can be controlled within 3 hours.

The impregnated silica gel powder has good drying performance, greatly shortens the drying time, and can shorten the drying time to 1H in a microwave drying environment because H can occur after plasma treatment₂0 → H.O.OH.OH.solution interface reaction is strengthened, and the movement frequency of water molecules is accelerated during drying.

Drawings

FIG. 1 is a scanning electron micrograph of a silica powder which has not been subjected to any treatment.

FIG. 2 is a scanning electron micrograph of the silica gel powder after the plasma treatment in example 1.

FIG. 3 is a scanning electron micrograph of a silicone powder which has not been plasma treated and has been further impregnated with ethyleneurea and polyethyleneimine.

Detailed Description

The invention is described in further detail below with reference to the accompanying examples.

Example 1:

40 parts of 100-mesh silica gel is placed in a plasma reaction chamber, treated by 100W low-temperature plasma for 20min under normal temperature and pressure oxygen flow, and taken out at normal temperature.

And secondly, in the process of the step 1), dissolving 5 parts of polyethyleneimine in 200 parts of deionized water, and dispersing by using a dispersing machine at a dispersion rotating speed of 20r/min for 5 min.

③ after the step 2) is finished, 15 parts of ethylene urea is dissolved in the mixed solution of the step 2), and a dispersion machine is used for dispersion, wherein the dispersion rotating speed is 20r/min, and the dispersion time is 10 min.

Adding the silica gel powder treated by the plasma in the step 1) into the solution in the step 3) after the dispersion is finished, and continuously dispersing the mixed suspension for 3 hours at the dispersion rotating speed of 20 r/min.

Filtering the dispersed liquid through a 200-mesh gauze to leave silica gel powder which is effectively impregnated, putting the powder in a glass tray, drying in a microwave drying device with the drying power set to 1000W, and drying for 1h to obtain the silica gel powder which is efficiently impregnated with the ethylene urea and the polyethyleneimine. The powder has high formaldehyde adsorbing effect.

Sixthly, mixing 30 parts of dried powder with 10 parts of carboxymethyl cellulose and 10 parts of water, putting the mixture into a roller type granulator for granulation, and drying the mixture for 30min under the condition of hot air drying after granulation to obtain silica gel particles with high viscosity, high strength and wear resistance.

The impregnated silica gel powder has good drying performance, greatly shortens the drying time from 3H to 1H in a microwave drying environment because H can be generated after plasma treatment₂0 → H.O.OH.OH.solution interface reaction is strengthened, and the movement frequency of water molecules is accelerated during drying.

Observed by a scanning electron microscope, the figure 1 shows the silica powder without any treatment, and the diameter of the spherical object is 20-30 nm.

Example 2:

15 parts of 100-mesh silica gel is placed in a plasma reaction chamber, treated by 100W low-temperature plasma for 20min under normal temperature and pressure oxygen flow, and taken out at normal temperature.

And secondly, in the process of the step 1), dissolving 10 parts of polyethyleneimine in 200 parts of deionized water, and dispersing by using a dispersion machine at the dispersion rotating speed of 20r/min for 5 min.

③ after the step 2) is finished, 5 parts of ethylene urea is dissolved in the mixed solution of the step 2), and a dispersion machine is used for dispersion, wherein the dispersion rotating speed is 20r/min, and the dispersion time is 10 min.

Adding the silica gel powder treated by the plasma in the step 1) into the solution in the step 3) after the dispersion is finished, and continuously dispersing the mixed suspension for 3 hours at the dispersion rotating speed of 20 r/min.

Filtering the dispersed liquid through a 200-mesh gauze to leave silica gel powder which is effectively impregnated, putting the powder in a glass tray, drying in a microwave drying device with the drying power set to 1000W, and drying for 1h to obtain the silica gel powder which is efficiently impregnated with the ethylene urea and the polyethyleneimine. The powder has high formaldehyde adsorbing effect.

Sixthly, mixing 10 parts of dried powder with 5 parts of carboxymethyl cellulose and 5 parts of water, putting the mixture into a roller type granulator for granulation, and drying the mixture for 30min under the condition of hot air drying after granulation to obtain silica gel particles with high viscosity, high strength and wear resistance.

FIG. 2 is a scanning electron microscope result of the plasma-treated silica gel powder of example 1, which is further impregnated with ethyleneurea and polyethyleneimine, wherein the diameter of the spheres is 25-35 nm, which shows that the ethyleneurea and polyethyleneimine crystallize on the surface of the silica gel, uniformly spread on the surface of the silica gel powder, and the thickness is 2-3 nm. The results show that under the plasma treatment, the ethylene urea successfully grows on the surface of the material and is uniformly distributed, the dipping time is shortened from 12h before the pretreatment to 3h, and the dipping time is shortened.

Example 3:

15 parts of 100-mesh silica gel is placed in a plasma reaction chamber, treated by 100W low-temperature plasma for 20min under normal temperature and pressure oxygen flow, and taken out at normal temperature.

And secondly, in the process of the step 1), dissolving 10 parts of polyethyleneimine in 200 parts of deionized water, and dispersing by using a dispersion machine at the dispersion rotating speed of 20r/min for 5 min.

③ after the step 2) is finished, 5 parts of ammonium sulfate is dissolved in the mixed solution of the step 2), and a dispersion machine is used for dispersion, wherein the dispersion rotating speed is 20r/min, and the dispersion time is 10 min.

Adding the silica gel powder treated by the plasma in the step 1) into the solution in the step 3) after the dispersion is finished, and continuously dispersing the mixed suspension for 3 hours at the dispersion rotating speed of 20 r/min.

Filtering the dispersed liquid through a 200-mesh gauze to leave silica gel powder which is effectively impregnated, putting the powder in a glass disc, drying in a microwave drying device with the drying power set to 1000W for 1h to obtain the silica gel powder which is efficiently impregnated with ammonium sulfate and polyethyleneimine. The powder has high formaldehyde adsorbing effect.

Sixthly, mixing 10 parts of dried powder with 5 parts of carboxymethyl cellulose and 5 parts of water, putting the mixture into a roller type granulator for granulation, and drying the mixture for 30min under the condition of hot air drying after granulation to obtain silica gel particles with high viscosity, high strength and wear resistance.

Example 4:

15 parts of 100-mesh silica gel is placed in a plasma reaction chamber, treated by 100W low-temperature plasma for 20min under normal temperature and pressure oxygen flow, and taken out at normal temperature.

And secondly, in the process of the step 1), dissolving 10 parts of polyethyleneimine in 200 parts of deionized water, and dispersing by using a dispersion machine at the dispersion rotating speed of 20r/min for 5 min.

③ after the step 2), 5 parts of alanine is dissolved in the mixed solution in the step 2), and a dispersion machine is used for dispersion, wherein the dispersion rotating speed is 20r/min, and the dispersion time is 10 min.

Adding the silica gel powder treated by the plasma in the step 1) into the solution in the step 3) after the dispersion is finished, and continuously dispersing the mixed suspension for 3 hours at the dispersion rotating speed of 20 r/min.

Filtering the dispersed liquid through a 200-mesh gauze to leave silica gel powder which is effectively impregnated, putting the powder in a glass disc, drying in a microwave drying device with the drying power set to 1000W, and drying for 1h to obtain the silica gel powder which is efficiently impregnated with alanine and polyethyleneimine. The powder has high formaldehyde adsorbing effect.

Sixthly, mixing 10 parts of dried powder with 5 parts of carboxymethyl cellulose and 5 parts of water, putting the mixture into a roller type granulator for granulation, and drying the mixture for 30min under the condition of hot air drying after granulation to obtain silica gel particles with high viscosity, high strength and wear resistance.

Comparative example 1:

dissolving 5 parts of polyethyleneimine in 200 parts of deionized water, and dispersing by using a dispersion machine at a dispersion speed of 20r/min for 5 min.

And (2) after the step 1) is finished, dissolving 15 parts of ethylene urea in the mixed solution obtained in the step 1), and dispersing for 10min at a dispersion rotating speed of 20r/min by using a dispersing machine.

Thirdly, 40 parts of 100-mesh silica gel powder is added into the solution obtained in the step 2) after the dispersion is finished, and the mixed suspension is continuously dispersed for 3 hours at the dispersion rotating speed of 20 r/min.

And fourthly, filtering the dispersed liquid through a 200-mesh gauze to leave silica gel powder which is effectively soaked, putting the powder into a glass disc, and drying in microwave drying equipment with the drying power set to 1000W for 1 h.

Mixing 30 parts of dried powder with 10 parts of carboxymethyl cellulose and 10 parts of water, putting the mixture into a roller type granulator for granulation, and drying the mixture for 30min under the condition of hot air drying after granulation.

FIG. 3 shows the scanning electron microscope results of the silicone powder which is not treated by plasma and is impregnated with ethylene urea and polyethyleneimine, wherein a large amount of spherical objects are adhered on the surface of the silicone powder, concentrated crystallization occurs, the load is uneven, and the adsorption performance of the material is affected.

Comparative example 2:

dissolving 10 parts of polyethyleneimine in 200 parts of deionized water, and dispersing by using a dispersion machine at the dispersion speed of 20r/min for 5 min.

And (2) after the step 1) is finished, dissolving 5 parts of ethylene urea in the mixed solution obtained in the step 1), and dispersing for 10min at a dispersion rotating speed of 20r/min by using a dispersing machine.

③ adding 15 parts of 100-mesh silica gel powder into the solution obtained in the step 2), and continuously dispersing the mixed suspension for 3 hours at a dispersion speed of 20 r/min.

And fourthly, filtering the dispersed liquid through a 200-mesh gauze to leave silica gel powder which is effectively soaked, putting the powder into a glass disc, and drying in microwave drying equipment with the drying power set to 1000W for 1 h.

Mixing 10 parts of dried powder with 5 parts of carboxymethyl cellulose and 5 parts of water, putting the mixture into a roller type granulator for granulation, and drying the mixture for 30min under the condition of hot air drying after granulation.

The water content test is obtained by testing a powder water content tester; the pore volume and the specific surface area are measured by a specific surface area analyzer (BET specific surface area method); the wear resistance detection method is in accordance with GB/T12496.6-1999; the strength test method was according to HG-T2782-1996. The adsorption capacity was measured by the fixed bed adsorption capacity method.

The data show that the silica gel treated by the plasma has obviously increased pore volume and specific surface area, higher adsorption capacity, better bonding property and better strength and wear resistance of the manufactured particles.