CN101804335A - Preparation method of organic-inorganic porous composite material for absorbing carbon dioxide - Google Patents
Preparation method of organic-inorganic porous composite material for absorbing carbon dioxide Download PDFInfo
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Abstract
The invention relates to a preparation method of a organic-inorganic porous composite material for absorbing carbon dioxide, which comprises the following steps: adding hydrogen-containing methyl polysiloxane into anhydrous ethanol, adding alkaline solution, mixing for 20-24 hours, adding deionized water into the solution, mixing for 0.5-5 hour(s), adding ethyl orthosilicate, mixing for 1-6 hour(s) to obtaining Solution A, dissolving organic amine into ethanol, mixing for 1-3 hour(s) to obtaining Solution B, adding the Solution B into the Solution A, mixing 3-5 hours, keeping static and aging for 3-5 days to obtain gel, and drying the gel for 24-30 hours at the temperature of 80-100 DEG C to remove ethanol in the system, thereby obtaining the organic-inorganic porous composite material. The invention has the advantages of low desorption temperature and high adsorption capacity. Simultaneously, the invention needs no template removing agent, thereby saving the cost and achieving good thermal stability.
Description
Technical field
The present invention relates to a kind of preparation method of porous material of adsorbing carbon dioxide efficiently, specifically a kind of preparation method of organic-inorganic porous composite material of adsorbing carbon dioxide efficiently.
Background technology
At present, fossil fuel such as coal and oil accounts at present more than 85% of consumes energy in the world.In this century, this class A fuel A is dominate still.Yet, the burning of fossil fuel but to airborne release a large amount of carbon dioxide, make atmosphere form fearful greenhouse effects, existent environment of people has been brought disastrous effect.Therefore, must exploitation otherwise effective technique control emission of carbon-dioxide, and, have important significance for theories and practical significance undoubtedly to the exploitation of the adsorbent of carbon dioxide high selectivity and high-adsorption-capacity.
At present, carbon dioxide physisorption material commonly used such as zeolite, active carbon have bigger adsorption capacity to carbon dioxide at low temperatures, but the selectivity to carbon dioxide when other gases exist is relatively poor, and when temperature was higher than 30 ℃, its adsorbance descended obviously.
Chemical absorbing demonstrates higher selectivity to carbon dioxide and absorbs.At present, the adsorbent that is used for the chemical absorbing carbon dioxide adopts liquid amine, and its main component is the water-soluble diethanol amine of energy.Though it is fairly simple that this alkanolamine solution prepares, there are many shortcomings in it: the first, and this performance of the adsorbent is poor, and adsorption efficiency is low.The second, the weight of liquid amine adsorbent is big.The 3rd, at adsorption/desorption CO
2Process in the loss of amine is arranged, make regeneration cycle efficient low, environment is caused secondary pollution.
At present, a lot of people begin mesopore molecular sieve is used for absorbing carbon dioxide, and the mesoporous molecular sieve SBA-15 of the about 21nm of American's synthetic aperture is after the template agent micella in 550 ℃ of high-temperature roasting removal ducts, flooding gamma-aminopropyl-triethoxy-silane again, is 4.6wt% to the adsorbance of carbon dioxide
The Japan scientific research personnel introduces amino on mesoporous si molecular sieves SBA-15 and MCM-41 by similar step with chlorosilane.U.S. Song Chun-shan Mountain seminar introduces the MCM-41 that the template agent is removed in high-temperature roasting with polymine, and in the time of 75 ℃, the gained material reaches 13.3wt% to the adsorbance of carbon dioxide.
Yet all there are the following problems for these sorbing materials: adsorption effect is relatively poor, need introduce more amino in porous material, and manage to make these amido high degree of dispersion in mesoporous material, to improve adsorption capacity and to obtain the good adsorption effect; Carrier need be removed the template agent, has caused the waste of the energy and to the pollution of environment in the process of template agent is removed in roasting.
Summary of the invention
The preparation method of organic-inorganic porous composite material who the purpose of this invention is to provide the absorbing carbon dioxide of a kind of adsorption effect and Heat stability is good.
The present invention realizes by the following method:
(1) will gather methyl hydrogen-containing siloxane (PMHS) is added in the absolute ethyl alcohol, add alkaline solution then, stir 20～24h, reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully, deionized water is added in the above-mentioned solution, behind stirring 0.5～5h, add ethyl orthosilicate again, stir 1～6h, be designated as solution A, wherein: PMHS: absolute ethyl alcohol: alkaline solution: deionized water: ethyl orthosilicate=1.2～4g: 180～250ml: 0.1～1g: 0.5～2g: 12g;
Described alkaline solution is solution of potassium carbonate, sodium carbonate liquor, ammonia spirit, sodium hydroxide solution or potassium hydroxide solution.
(2) organic amine is dissolved in the ethanol, stirs 1～3h, organic amine is fully dissolved, obtain solution B, wherein: organic amine: ethanol=1.11g～2.77g: 10～20ml;
Described organic amine is one or more the mixture in triethylene diamine, diethanol amine, diethylenetriamine, the polymine.
(3) solution B is joined in the solution A, after stirring 3～5h, leaving standstill wears out obtained gel after 3～5 days, the gel of gained is placed on dry 24～30h under 80～100 ℃ of temperature, remove the ethanol in the system, obtain organic-inorganic porous composite material, the proportioning between solution B and the solution A is pressed organic amine: ethyl orthosilicate=0.5g～4.55g: 12g.
The present invention compared with prior art has following advantage:
1, in order to improve adsorption effect, in porous material, introduces organic amine by synthetic method of a step, and these organic amines evenly are coated on the porous material surface.
2, utilize high efficiency interaction between organic amine and the carbon dioxide molecule to realize the efficient absorption of carbon dioxide, utilize the organic-inorganic porous composite material of this method preparation not only to have low desorption temperature, higher adsorbance, simultaneously do not need to remove the template agent, provide cost savings good heat endurance.
The specific embodiment
The adsorbance of gravimetric detemination carbon dioxide: get the 100mg sample and pack in the quartz boat, read the length of quartz spring elongation, at vacuum state (10
-2Pa, 200 ℃) handle sample 2h down, when treating that temperature is reduced to 30 ℃, write down the residing scale of spring this moment, in system, slowly feed carbon dioxide, to treat to write down the residing scale of spring once more after the adsorption equilibrium, the difference of twice record is scaled the sample CO absorption
2Weight.
Embodiment 1:
1.2g PMHS is added drop-wise in the triangular flask of 180ml absolute ethyl alcohol, adds alkaline solution then, stir 20h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 0.5g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 0.5h, drips the ethyl orthosilicate of 12g again.Stir 1h, be designated as solution A.The 1.70g polymine is dissolved in the ethanol of 10ml, stirs 1h, polymine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 3h, leaving standstill wears out obtained gel after 3 days.Gel dry 24h in 80 ℃ baking oven with gained removes the ethanol in the system, obtains the sample that the polyethyleneimine: amine content is 30wt%, is designated as S1-30, utilizes gravimetric method to record the adsorbance data, and its adsorbance data see Table 1.
Embodiment 2:
1.2g PMHS is added drop-wise in the triangular flask of 180ml absolute ethyl alcohol, adds alkaline solution then, stir 20h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 0.5g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 0.5h, drips the ethyl orthosilicate of 12g again.Stir 1h, be designated as solution A.The 2.26g polymine is dissolved in the ethanol of 10ml, stirs 1h, polymine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 3h, leaving standstill wears out obtained gel after 3 days.Gel dry 24h in 80 ℃ baking oven with gained removes the ethanol in the system, obtains the sample that the polyethyleneimine: amine content is 40wt%, is designated as S1-40.Utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 1.
Embodiment 3:
1.2g PMHS is added drop-wise in the triangular flask of 180ml absolute ethyl alcohol, adds alkaline solution then, stir 20h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 0.5g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 0.5h, drips the ethyl orthosilicate of 12g again.Stir 1h, be designated as solution A.The 2.83g polymine is dissolved in the ethanol of 10ml, stirs 1h, polymine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 3h, leaving standstill wears out obtained gel after 3 days.Gel dry 24h in 80 ℃ baking oven with gained removes the ethanol in the system, obtains the sample that the polyethyleneimine: amine content is 50wt%, is designated as S1-50, utilizes gravimetric method to record the adsorbance data, and its adsorbance data see Table 1.
Embodiment 4:
1.5g PMHS is added drop-wise in the triangular flask of 200ml absolute ethyl alcohol, and then adds alkaline solution, stir 22h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 0.75g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 0.5h, drips the ethyl orthosilicate of 12g again.Stir 1.5h, be designated as solution A.The 1.66g triethylene diamine is dissolved in the ethanol of 12ml, stirs 1.5h, triethylene diamine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 4h, leaving standstill wears out obtained gel after 3 days.Gel dry 24h in 90 ℃ baking oven with obtaining removes the ethanol in the system, obtains the sample that triethylene diamine content is 30wt%, is designated as S2-30.Utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 2.
Embodiment 5:
1.5g PMHS is added drop-wise in the triangular flask of 200ml absolute ethyl alcohol, and then adds alkaline solution, stir 22h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 0.75g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 0.5h, drips the ethyl orthosilicate of 12g again.Stir 1.5h, be designated as solution A.The 2.22g triethylene diamine is dissolved in the ethanol of 12ml, stirs 1.5h, triethylene diamine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 4h, leaving standstill wears out obtained gel after 3 days.Gel dry 24h in 90 ℃ baking oven with obtaining removes the ethanol in the system, obtains the sample that triethylene diamine content is 40wt%, is designated as S2-40.Utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 2.
Embodiment 6:
1.5g PMHS is added drop-wise in the triangular flask of 200ml absolute ethyl alcohol, and then adds alkaline solution, stir 22h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 0.75g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 0.5h, drips the ethyl orthosilicate of 12g again.Stir 1.5h, be designated as solution A.The 2.77g triethylene diamine is dissolved in the ethanol of 12ml, stirs 1.5h, triethylene diamine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 4h, leaving standstill wears out obtained gel after 3 days.Gel dry 24h in 90 ℃ baking oven with obtaining removes the ethanol in the system, obtains the sample that triethylene diamine content is 50wt%, is designated as S2-50.Utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 2.
Embodiment 7:
1.8g PMHS is added drop-wise in the triangular flask of 210ml absolute ethyl alcohol, and then adds alkaline solution, stir 23h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 1.0g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 1h, drips the ethyl orthosilicate of 12g again.Stir 2h, be designated as solution A.The 1.66g diethanol amine is dissolved in the ethanol of 13ml, stirs 2h, diethanol amine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 4h, leaving standstill wears out obtained gel after 4 days.Gel dry 24h in 90 ℃ baking oven with obtaining removes the ethanol in the system, obtains the sample that diethanol amine content is 30wt%, is designated as S3-30, utilizes gravimetric method to record the adsorbance data, and its adsorbance data see Table 3.
Embodiment 8:
1.8g PMHS is added drop-wise in the triangular flask of 210ml absolute ethyl alcohol, and then adds alkaline solution, stir 23h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 1.0g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 1h, drips the ethyl orthosilicate of 12g again.Stir 2h, be designated as solution A.The 2.21g diethanol amine is dissolved in the ethanol of 13ml, stirs 2h, diethanol amine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 4h, leaving standstill wears out obtained gel after 4 days.Gel dry 24h in 90 ℃ baking oven with obtaining removes the ethanol in the system, obtains the sample that diethanol amine content is 40wt%, is designated as S3-40, utilizes gravimetric method to record the adsorbance data, and its adsorbance data see Table 3.
Embodiment 9:
1.8g PMHS is added drop-wise in the triangular flask of 210ml absolute ethyl alcohol, and then adds alkaline solution, stir 23h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 1.0g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 1h, drips the ethyl orthosilicate of 12g again.Stir 2h, be designated as solution A.The 2.77g diethanol amine is dissolved in the ethanol of 13ml, stirs 2h, diethanol amine is fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 4h, leaving standstill wears out obtained gel after 4 days.Gel dry 24h in 90 ℃ baking oven with obtaining removes the ethanol in the system, obtains the sample that diethanol amine content is 50wt%, is designated as S3-50.Utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 3.
Embodiment 10:
3g PMHS is added drop-wise in the triangular flask of 240ml absolute ethyl alcohol, and then adds alkaline solution, stir 24h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 1.75g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 2h, drips the ethyl orthosilicate of 12g again.Stir 2.5h, be designated as solution A.1.11g diethylenetriamine and 1.11g diethanol amine are dissolved in the ethanol of 18ml, stir 2.5h, diethylenetriamine and diethanol amine are fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 5h, leaving standstill wears out obtained gel after 5 days.With the gel dry 30h in 100 ℃ baking oven that obtains, remove the ethanol in the system, the weight percentage of diethylenetriamine and diethanol amine is respectively 20% and 10% in the gained sample, is designated as S4-20-10, utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 4.
Embodiment 11:
3g PMHS is added drop-wise in the triangular flask of 240ml absolute ethyl alcohol, and then adds alkaline solution, stir 24h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 1.75g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 2h, drips the ethyl orthosilicate of 12g again.Stir 2.5h, be designated as solution A.1.66g diethylenetriamine and 1.11g diethanol amine are dissolved in the ethanol of 18ml, stir 2.5h, diethylenetriamine and diethanol amine are fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 5h, leaving standstill wears out obtained gel after 5 days.With the gel dry 30h in 100 ℃ baking oven that obtains, remove the ethanol in the system, the weight percentage of diethylenetriamine and diethanol amine is respectively 30% and 10% in the gained sample, is designated as S4-30-10, utilize gravimetric method to record the adsorbance data, its adsorbance data see Table 4.
Embodiment 12:
4g PMHS is added drop-wise in the triangular flask of 250ml absolute ethyl alcohol, and then adds alkaline solution, stir 24h, the reactive hydrogen atom on the PMHS molecule is replaced by ethyoxyl fully.The 2g deionized water is added drop-wise in the above-mentioned solution, behind the stirring 2h, drips the ethyl orthosilicate of 12g again.Stir 3h, be designated as solution A.2.21g diethylenetriamine and 1.11g diethanol amine are dissolved in the ethanol of 20ml, stir 3h, diethylenetriamine and triethylene diamine are fully dissolved, obtain solution B.Solution B is joined in the solution A, and behind the stirring 5h, leaving standstill wears out obtained gel after 5 days.Gel dry 24h in 100 ℃ baking oven with obtaining removes the ethanol in the system, obtains block white transparent solid.The weight percentage of diethylenetriamine and triethylene diamine is respectively 40% and 10% in the gained sample, is designated as S4-40-10, utilizes gravimetric method to record the adsorbance data, and its adsorbance data see Table 4.
The carbon dioxide adsorption data of table 1:S1-polymine composite
| Sample | ??CO 2Adsorbance (mg/g) |
| ??S2-30％ | ??38.2 |
| ??S2-40％ | ??49 |
| ??S2-50％ | ??98 |
The carbon dioxide adsorption data of table 2:S2-triethylene diamine composite
| Sample | ??CO 2Adsorbance (mg/g) |
| ??S3-30％ | ??37 |
| ??S3-40％ | ??45 |
| ??S3-50％ | ??89 |
The carbon dioxide adsorption data of table 3:S3-diethanol amine composite
| Sample | ??CO 2Adsorbance (mg/g) |
| ??S3-30％ | ??48.1 |
| ??S3-40％ | ??55 |
| ??S3-50％ | ??105 |
The carbon dioxide adsorption data of table 4:S4-m-n-diethylenetriamine and diethanol amine composite
| Sample | ??CO 2Adsorbance (mg/g) |
| ??S4-20％-10％ | ??41 |
| ??S4-30％-10％ | ??50 |
| ??S4-40％-10％ | ??92 |
Claims (3)
1. the preparation method of the organic-inorganic porous composite material of an absorbing carbon dioxide is characterized in that comprising the steps:
(1) will gather the methyl hydrogen-containing siloxane is added in the absolute ethyl alcohol, add alkaline solution then, stir 20～24h, deionized water is added in the above-mentioned solution, after stirring 0.5～5h, add ethyl orthosilicate again, stir 1～6h, be designated as solution A, wherein: poly-methyl hydrogen-containing siloxane: absolute ethyl alcohol: alkaline solution: deionized water: ethyl orthosilicate=1.2～4g: 180～250ml: 0.1～1g: 0.5～2g: 12g;
(2) organic amine is dissolved in the ethanol, stirs 1～3h, organic amine is fully dissolved, obtain solution B, wherein: organic amine: ethanol=1.11g～2.77g: 10～20ml;
(3) solution B is joined in the solution A, after stirring 3～5h, leaving standstill wears out obtained gel after 3～5 days, the gel of gained is placed on dry 24～30h under 80～100 ℃ of temperature, remove the ethanol in the system, obtain organic-inorganic porous composite material, the proportioning between solution B and the solution A is pressed organic amine: ethyl orthosilicate=0.5g～4.55g: 12g.
2. the preparation method of the organic-inorganic porous composite material of a kind of absorbing carbon dioxide as claimed in claim 1 is characterized in that described alkaline solution is solution of potassium carbonate, sodium carbonate liquor, ammonia spirit, sodium hydroxide solution or potassium hydroxide solution.
3. the preparation method of the organic-inorganic porous composite material of a kind of absorbing carbon dioxide as claimed in claim 1 is characterized in that described organic amine is one or more the mixture in triethylene diamine, diethanol amine, diethylenetriamine, the polymine.
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