CN113429943B - Modified attapulgite and preparation method of modified attapulgite-based composite phase change material - Google Patents
Modified attapulgite and preparation method of modified attapulgite-based composite phase change material Download PDFInfo
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Abstract
The invention discloses a modified attapulgite and a preparation method of a modified attapulgite-based composite phase change material, wherein the preparation method of the modified attapulgite-based composite phase change material comprises the following steps: (1) alkali activation modification: reacting attapulgite raw ore with alkali liquor to perform alkali activation modification to obtain alkali-modified attapulgite; (2) and (3) calcining: calcining the alkali-modified attapulgite; (3) acid activation modification: reacting the calcined attapulgite with acid liquor to perform acid activation modification, and obtaining modified attapulgite after modification; (4) adsorption: and adsorbing the phase change material by using the modified attapulgite as a carrier to obtain the modified attapulgite composite phase change material. According to the invention, the attapulgite is modified by adopting alkali activation modification, calcination and acid activation modification processes, so that the adsorption capacity of the attapulgite can be obviously improved, and then the composite phase change material is prepared by taking the modified attapulgite as a carrier and taking the organic phase change material as an adsorption object, so that the obtained composite phase change material has high latent heat, low cost and excellent performance.
Description
Technical Field
The invention relates to the technical field of modified materials, in particular to a modified attapulgite and a preparation method of a modified attapulgite-based composite phase change material.
Background
The organic phase-change material can adjust the external temperature through the reversible phase-change process of melting-solidification, thereby realizing the purposes of energy conservation and emission reduction. The organic phase-change material has the characteristics of high phase-change latent heat and good thermal stability, and can be used in the fields of solar energy utilization, industrial waste heat recovery, electronic device temperature control and the like. However, the organic phase-change material has a leakage problem, so that the phase-change material flows to cause loss, and the heat storage performance is degraded. Therefore, the organic phase change material is usually packaged to prepare a composite phase change material, so as to overcome the problem that the organic phase change material is easy to leak.
As a natural one-dimensional nano material, attapulgite is a silicate clay mineral in a chain layer shape, and has larger specific surface area, rich pore structure and nano rod/fiber shape in microscopic appearance. The attapulgite is widely distributed in the world, has huge reserves, is natural and pollution-free, and is an ideal choice as a phase change material carrier. The attapulgite crude ore has low loading capacity on the organic phase change material, and the reason is that the staggered pore structure of the attapulgite fibers is blocked by impurities such as organic matters, carbonate and the like. The attapulgite does not change before and after phase change, the specific heat capacity is small, and almost no heat is transferred, and the phase change material absorbs or releases a large amount of heat before and after phase change, so that the higher the specific gravity of the phase change material in the attapulgite-based composite phase change material is, the higher the latent heat of the phase change material is, and the better the heat storage performance is. Meanwhile, the attapulgite is pretreated, and the removal of impurities in pores is the key for improving the adsorption capacity of the attapulgite on the phase-change material and improving the energy storage density of the attapulgite-based composite phase-change material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a modified attapulgite and a preparation method of the modified attapulgite-based composite phase change material, wherein the modified attapulgite is modified by adopting the processes of alkali activation modification, calcination and acid activation modification, so that the specific surface area and the pore volume of the attapulgite are improved, the loading capacity of the attapulgite on an organic phase change material is improved, the modified attapulgite is used as a carrier, the organic phase change material is used as an adsorption object to prepare the attapulgite-based composite phase change material, and the energy storage density of the composite material is finally improved.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of the modified attapulgite comprises the following steps:
(1) alkali activation modification: reacting attapulgite raw ore with alkali liquor to perform alkali activation modification to obtain alkali-modified attapulgite;
(2) and (3) calcining: calcining the alkali-modified attapulgite;
(3) acid activation modification: and reacting the calcined attapulgite with acid liquor to perform acid activation modification, and obtaining the modified attapulgite after modification.
As a further improvement of the scheme, the alkali liquor comprises one or more of sodium hydroxide solution and potassium hydroxide solution, the mass concentration of the alkali liquor is 5-10%, the dosage of the alkali liquor is 3-10 times of the mass of the attapulgite raw ore, the activation temperature is 40-80 ℃ and the activation time is 1-4 hours during alkali activation modification.
As a further improvement of the scheme, the calcining treatment temperature is 100-300 ℃, and the calcining time is 1-24 h.
As a further improvement of the scheme, the acid solution comprises one or more of sulfuric acid, hydrochloric acid and nitric acid, the mass concentration of the acid solution is 5-30%, the using amount of the acid solution is 3-10 times of the mass of the calcined attapulgite, the activation temperature is 40-80 ℃ and the activation time is 1-4 hours during acid activation modification.
The second aspect of the invention is to provide a modified attapulgite which is used as a carrier of an attapulgite-based composite phase change material and is prepared by the preparation method of the modified attapulgite.
The third aspect of the invention provides a preparation method of a modified attapulgite-based composite phase-change material, which comprises the following steps:
(1) alkali activation modification: reacting attapulgite raw ore with alkali liquor to perform alkali activation modification to obtain alkali-modified attapulgite;
(2) and (3) calcining: calcining the alkali-modified attapulgite;
(3) acid activation modification: reacting the calcined attapulgite with acid liquor to perform acid activation modification, and obtaining modified attapulgite after modification;
(4) adsorption: and adsorbing the phase change material by using the modified attapulgite as a carrier to obtain the modified attapulgite composite phase change material.
As a further improvement of the scheme, the alkali liquor comprises one of sodium hydroxide solution and potassium hydroxide solution, the mass concentration of the alkali liquor is 5-10%, the dosage of the alkali liquor is 3-10 times of the mass of the attapulgite raw ore, the activation temperature is 40-80 ℃ and the activation time is 1-4 hours during alkali activation modification.
As a further improvement of the scheme, the calcining treatment temperature is 100-300 ℃, and the calcining time is 1-24 h.
As a further improvement of the scheme, the acid solution comprises one or more of sulfuric acid, hydrochloric acid and nitric acid, the mass concentration of the acid solution is 5-30%, the using amount of the acid solution is 3-10 times of the mass of the calcined attapulgite, the activation temperature is 40-80 ℃ and the activation time is 1-4 hours during acid activation modification.
As a further improvement of the scheme, the phase change material comprises one or more of paraffin, stearic acid and polyethylene glycol.
As a further improvement of the scheme, when the modified attapulgite is used as a carrier to adsorb the phase change material, an impregnation method or a vacuum impregnation method can be adopted.
As a further improvement of the above scheme, the impregnation method specifically comprises: soaking the modified attapulgite serving as a carrier in a soluble solution of the phase-change material, and separating residual liquid after contacting for a certain time to obtain the modified attapulgite-based composite phase-change material.
As a further improvement of the above scheme, the vacuum impregnation method is the same as the impregnation method in step, except that the vacuum method is adopted to evacuate air in the pores inside the substrate and then the impregnation treatment is carried out, so that the impregnant quickly permeates into the pores and is completely filled.
Compared with the prior art, the invention has the beneficial effects that:
the modified attapulgite-based composite phase change material has the advantages of low cost, high latent heat and excellent performance.
In summary, in order to improve the specific surface area and the pore volume of the attapulgite and improve the loading capacity of the attapulgite on organic phase change materials, the invention adopts a combined process of alkali activation modification, calcination and acid activation modification to modify the attapulgite according to the process sequence, wherein the alkali activation modification can change the pore canals of the attapulgite and increase the specific surface area in a small range, and meanwhile, the alkali activation treatment can dissolve S i-O tetrahedrons at the tail end of the attapulgite, thereby forming amorphous MgO and FeOx aggregation; the purpose of calcination is mainly to remove adsorbed water and bound water in the crystal structure of attapulgite; the acid activation modification aims at dissolving organic matters, carbonate and other impurities in the staggered pore structure of the attapulgite fiber and has the function of dredging pore channels; and finally, preparing the modified attapulgite-based composite phase change material with excellent performance by taking the modified attapulgite as a carrier and the organic phase change material as an adsorption object.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1:
a preparation method of the modified attapulgite-based composite paraffin phase-change material comprises the following steps:
(1) weighing 500g of attapulgite raw ore, adding 5000g of sodium hydroxide solution with the concentration of 5%, uniformly mixing, and reacting at 50 ℃ for 4h to obtain alkali-modified attapulgite;
(2) filtering and washing the alkali-modified attapulgite until the attapulgite is neutral, drying and crushing the attapulgite, and calcining the attapulgite at the temperature of 300 ℃ for 1 h;
(3) adding 2000g of 5% sulfuric acid solution into 200g of calcined attapulgite powder, mixing, reacting at 80 deg.C for 1 hr, filtering the attapulgite powder, washing to neutral, oven drying at 105 deg.C to constant weight, pulverizing to obtain particle size, and sieving with 200 mesh sieve to obtain modified attapulgite;
(4) and adding 100g of paraffin into 100g of modified attapulgite, stirring for 24 hours at 60 ℃, and then performing suction filtration at 60 ℃ to remove redundant paraffin to obtain the modified attapulgite-based composite paraffin phase-change material.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared by the embodiment is 96.1J/g.
Example 2:
a preparation method of a modified attapulgite-based composite stearic acid phase-change material comprises the following steps:
(1) weighing 300g of attapulgite raw ore, adding 900g of 10% potassium hydroxide solution, mixing uniformly, and reacting at 40 ℃ for 2h to obtain alkali-modified attapulgite;
(2) filtering and washing the alkali-modified attapulgite until the attapulgite is neutral, drying and crushing the attapulgite, and calcining the attapulgite at the temperature of 100 ℃ for 24 hours;
(3) taking 150g of calcined attapulgite powder, adding 450g of hydrochloric acid solution with the concentration of 30%, uniformly mixing, reacting at 40 ℃ for 4h, filtering and washing the attapulgite powder to be neutral after the reaction is finished, drying at 105 ℃ to constant weight, crushing to obtain the particle size, and sieving with a 200-mesh sieve to obtain the modified attapulgite;
(4) taking 100g of modified attapulgite, adding 150g of stearic acid, stirring at 80 ℃ for 24h, and then filtering at 80 ℃ to remove redundant stearic acid to obtain the modified attapulgite-based composite stearic acid phase-change material.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared in the embodiment is 76.1J/g.
Example 3:
a preparation method of a modified attapulgite-based composite polyethylene glycol phase-change material comprises the following steps:
(1) weighing 400g of attapulgite raw ore, adding 400g of 5% sodium hydroxide solution and 1200g of 10% potassium hydroxide solution, stirring and mixing uniformly, and reacting at 60 ℃ for 3h to obtain alkali-modified attapulgite;
(2) filtering and washing the alkali-modified attapulgite until the attapulgite is neutral, drying and crushing the attapulgite, and calcining the attapulgite at 200 ℃ for 3 hours;
(3) adding 400g of 10% sulfuric acid solution and 400g of 10% nitric acid solution into 200g of calcined attapulgite powder, stirring and mixing uniformly, reacting at 60 ℃ for 3h, filtering and washing the attapulgite powder to be neutral after the reaction is finished, drying at 105 ℃ to constant weight, crushing to obtain particles, and sieving with a 200-mesh sieve to obtain the modified attapulgite;
(4) taking 100g of modified attapulgite, adding 120g of polyethylene glycol, stirring at 80 ℃ for 24h, and then filtering at 80 ℃ to remove redundant polyethylene glycol to obtain the modified attapulgite-based composite polyethylene glycol phase-change material.
The phase change latent heat of the modified attapulgite-based composite polyethylene glycol phase change material prepared by the embodiment is 86.4J/g.
Example 4:
a preparation method of the modified attapulgite-based composite paraffin phase-change material comprises the following steps:
(1) weighing 500g of attapulgite raw ore, adding 2500g of 10% sodium hydroxide solution, mixing uniformly, and reacting at 80 ℃ for 4h to obtain alkali-modified attapulgite;
(2) filtering and washing the alkali-modified attapulgite until the attapulgite is neutral, drying and crushing the attapulgite, and calcining the attapulgite at the temperature of 300 ℃ for 4 hours;
(3) adding 1000g of 5% sulfuric acid solution into 200g of calcined attapulgite powder, mixing, reacting at 80 deg.C for 3h, filtering the attapulgite powder, washing to neutral, oven drying at 105 deg.C to constant weight, pulverizing to obtain particle size, and sieving with 200 mesh sieve to obtain modified attapulgite;
(4) taking 100g of modified attapulgite, adding 120g of paraffin, stirring for 24h at 60 ℃, then transferring into a vacuum drying oven, vacuumizing at 60 ℃, standing for 12h, and then performing suction filtration to remove redundant paraffin to obtain the modified attapulgite-based composite paraffin phase-change material.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared by the embodiment is 101.1J/g.
Comparative example 1:
the preparation method of the modified attapulgite-based composite paraffin phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those in the embodiment 1, except that: omitting the step (1), and directly calcining the attapulgite raw ore and then performing acid activation treatment.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared in the comparative example 1 is 74.78J/g.
Comparative example 2:
the preparation method of the modified attapulgite-based composite paraffin phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those in the embodiment 1, except that: omitting the step (2), and directly carrying out acid activation treatment modification on the attapulgite subjected to alkali activation modification without calcining.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared in the comparative example 2 is 82.32J/g.
Comparative example 3:
the preparation method of the modified attapulgite-based composite paraffin phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those in the embodiment 1, except that: and (4) omitting the step (3), calcining the attapulgite subjected to alkali activation modification, and directly preparing the composite phase change material without acid activation modification after calcination.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared in the comparative example 3 is 76.44J/g.
Comparative example 4:
the preparation method of the modified attapulgite-based composite paraffin phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those in the embodiment 1, except that: and (4) sequentially replacing the step (1) and the step (3), namely, firstly carrying out acid activation modification on the attapulgite raw ore, and then carrying out alkali activation modification after calcination.
The phase change latent heat of the modified attapulgite-based composite paraffin phase change material prepared in the comparative example 4 is 70.56J/g.
Comparative example 5:
the preparation method of the modified attapulgite-based composite stearic acid phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those of the example 2, except that: omitting the step (1), and directly calcining the attapulgite raw ore and then performing acid activation treatment.
The phase change latent heat of the modified attapulgite-based composite stearic acid phase change material prepared in the comparative example 5 is 71.2J/g.
Comparative example 6:
the preparation method of the modified attapulgite-based composite stearic acid phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those of the example 2, except that: omitting the step (2), and directly carrying out acid activation treatment modification on the attapulgite subjected to alkali activation modification without calcining.
The phase change latent heat of the modified attapulgite-based composite stearic acid phase change material prepared in the comparative example 6 is 73.2J/g.
Comparative example 7:
the preparation method of the modified attapulgite-based composite stearic acid phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those of the example 2, except that: and (4) omitting the step (3), calcining the attapulgite subjected to alkali activation modification, and directly preparing the composite phase change material without acid activation modification after calcination.
The phase change latent heat of the modified attapulgite-based composite stearic acid phase change material prepared in the comparative example 7 is 68.7J/g.
Comparative example 8:
the preparation method of the modified attapulgite-based composite stearic acid phase-change material comprises the following steps of the steps, and the process parameters of the steps are the same as those of the example 2, except that: and (3) sequentially replacing the steps (1) and (3), namely, firstly carrying out acid activation modification on the attapulgite raw ore, and then carrying out alkali activation modification after calcining.
The phase change latent heat of the modified attapulgite-based composite stearic acid phase change material prepared in the comparative example 8 is 69.8J/g.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (1)
1. The preparation method of the modified attapulgite-based composite phase change material is characterized by comprising the following steps of:
(1) alkali activation modification: reacting attapulgite raw ore with alkali liquor to perform alkali activation modification to obtain alkali-modified attapulgite; the alkali liquor comprises one of sodium hydroxide solution and potassium hydroxide solution, the mass concentration of the alkali liquor is 5-10%, the dosage of the alkali liquor is 3-10 times of the mass of attapulgite raw ore, the activation temperature is 40-80 ℃ and the activation time is 1-4 h during alkali activation modification;
(2) and (3) calcining: calcining the alkali-modified attapulgite; the calcining temperature is 100-300 ℃, and the calcining time is 1-24 h;
(3) acid activation modification: reacting the calcined attapulgite with acid liquor to perform acid activation modification, and obtaining modified attapulgite after modification; the acid solution comprises one or more of sulfuric acid, hydrochloric acid and nitric acid, the mass concentration of the acid solution is 5-30%, the using amount of the acid solution is 3-10 times of the mass of the calcined attapulgite, the activation temperature is 40-80 ℃ and the activation time is 1-4 hours during acid activation modification;
(4) adsorption: adsorbing the phase change material by using the modified attapulgite as a carrier to obtain a modified attapulgite composite phase change material; the phase change material comprises one or more of paraffin, stearic acid and polyethylene glycol.
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