CN104058402A - Method of preparing high purity carbon dioxide - Google Patents

Method of preparing high purity carbon dioxide Download PDF

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Publication number
CN104058402A
CN104058402A CN201410265632.0A CN201410265632A CN104058402A CN 104058402 A CN104058402 A CN 104058402A CN 201410265632 A CN201410265632 A CN 201410265632A CN 104058402 A CN104058402 A CN 104058402A
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carbon dioxide
metal ion
purity carbon
preparing high
sieve
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CN201410265632.0A
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CN104058402B (en
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张建中
佟天宇
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Fushun Vocationl Technical College
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Fushun Vocationl Technical College
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    • Y02P20/121

Abstract

The invention belongs to the technical field of extraction and purification and particularly relates to a method of preparing high purity carbon dioxide. The method is a process method of preparing high purity carbon dioxide by adopting a polymetal ion modified phosphorus-aluminum framework molecular sieve. The method provided by the invention comprises the following steps: firstly, synthesizing the metal ion modified phosphorus-aluminum framework molecular sieve; then, by taking the sieve as an adsorbent to adsorb and remove impurities in a raw material carbon dioxide, thus obtaining high purity carbon dioxide by inspecting the reaction temperature, the reaction pressure and the airspeed value in the adsorption process, wherein finally, the purity of the prepared carbon dioxide can reach 99.999%, and the effect is remarkable. The method of preparing high purity carbon dioxide by adopting the metal ion modified phosphorus-aluminum framework molecular sieve provided by the invention is less in used equipment, small in occupied area, energy-saving and cost-lowering and has an extremely good social benefit in the aspects such as resource and energy conservation, environmental protection and the like.

Description

A kind of method of preparing high-purity carbon dioxide
Technical field
The invention belongs to purifying technical field, be specifically related to a kind of method of preparing high-purity carbon dioxide, is to adopt the processing method of how metal ion-modified phosphorus aluminium molecule of the skeleton sieve series for high-purity carbon dioxide.
Background technology
Carbonic acid gas is important industrial production raw material, be widely used in the fields such as metallurgy, iron and steel, oil, chemical industry, electronics, food, medical treatment, have been widely used at aspect tools such as industrial application especially, application, the supercritical extraction etc. of drink industry, so it is extremely important to prepare highly purified carbonic acid gas.Be applied at present carbonic acid gas purifying be mainly oxidation, absorption, the conventional steps such as distillation, exist use equipment many, floor space is large, consume energy high, efficiency low with high in cost of production problem.
Summary of the invention
The object of this invention is to provide a kind of method of preparing high-purity carbon dioxide, is to adopt the processing method of how metal ion-modified phosphorus aluminium molecule of the skeleton sieve series for high-purity carbon dioxide.Adopt the analysis of metal ion-modified phosphorus aluminium skeleton to sieve synthesis carbonic acid gas; purity to 99.999%; the method is integrated several technological processs; minimizing equipment, floor space and operator, the saving energy, reduce costs; more effective than traditional thinking and method, economizing on resources and the aspect such as the energy, environment protection has great social benefit.There is great scientific meaning and social application prospect.
The solution of the present invention is:
A method of preparing high-purity carbon dioxide, comprising:
Sieve as sorbent material taking metal ion-modified phosphorus aluminium molecule of the skeleton, the impurity in feed carbon dioxide is removed in absorption, and to obtain high-purity carbon dioxide, wherein, described metal ion is the one being selected from IB, IIIB and VIII family element.
Preferably, in the described method of preparing high-purity carbon dioxide, described metal ion is nickel, copper, iron, cerium or silver element.
Preferably, in the described method of preparing high-purity carbon dioxide, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of metal ion is 3%.
Preferably, in the described method of preparing high-purity carbon dioxide, described metal ion is ferro element.
Preferably, in the described method of preparing high-purity carbon dioxide, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of ferro element is 9%.
Preferably, in the described method of preparing high-purity carbon dioxide, adsorption conditions is: 25 DEG C of temperature, pressure 3.5MPa, air speed 80min -1.
Preferably, in the described method of preparing high-purity carbon dioxide, the particle diameter of described metal ion-modified phosphorus aluminium molecule of the skeleton sieve is 60~80 μ m.
Preferably, in the described method of preparing high-purity carbon dioxide, adopt equi-volume impregnating to prepare described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, wherein, the metal ion aqueous solution taking mass concentration as 3~15% is as steeping fluid, and dipping time is 10~100min.
Beneficial effect of the present invention is:
1. carbon dioxide purity reaches more than 99.999%.
2. foreign gas content is little: hydrogen (H2) content≤0.5% (volume ratio), oxygen content≤1% (volume ratio), a nitrogen content≤3% (volume ratio), carbon monoxide content≤0.5% (volume ratio), total hydrocarbon (THC) content≤2% (volume ratio), moisture content≤2% (volume ratio).
3. whole building-up process is pollution-free to surrounding environment.
Brief description of the drawings
Fig. 1 is the metal ion-modified phosphorus aluminium molecule of the skeleton sieve data results of adsorption selectivity the best;
Fig. 2 is the investigation data results to air speed adsorption conditions.
Embodiment
The present invention is described in further detail below, to make those skilled in the art can implement according to this with reference to specification sheets word.
A method of preparing high-purity carbon dioxide, comprising:
Sieve as sorbent material taking metal ion-modified phosphorus aluminium molecule of the skeleton, the impurity in feed carbon dioxide is removed in absorption, and to obtain high-purity carbon dioxide, wherein, described metal ion is the one being selected from IB, IIIB and VIII family element.
In the described method of preparing high-purity carbon dioxide, described metal ion is nickel, copper, iron, cerium or silver element.
In the described method of preparing high-purity carbon dioxide, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of metal ion is 3%.
In the described method of preparing high-purity carbon dioxide, described metal ion is ferro element.
Preferably, in the described method of preparing high-purity carbon dioxide, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of ferro element is 9%.
In the described method of preparing high-purity carbon dioxide, adsorption conditions is: 25 DEG C of temperature, pressure 3.5MPa, air speed 80min -1.
In the described method of preparing high-purity carbon dioxide, the particle diameter of described metal ion-modified phosphorus aluminium molecule of the skeleton sieve is 60~80 μ m.
In the described method of preparing high-purity carbon dioxide, adopt equi-volume impregnating to prepare described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, wherein, the metal ion aqueous solution taking mass concentration as 3~15% is as steeping fluid, and dipping time is 10~100min.
Prepare respectively nickelous nitrate, cupric nitrate, iron nitrate, cerous nitrate and the Silver Nitrate steeping fluid of 1M, make the metal ions such as nickel, copper, iron, cerium and silver carry out modification to phosphorus aluminium molecule of the skeleton sieve, charge capacity and the particle diameter of five metal ion species are as shown in table 1, under identical adsorption conditions, prepare respectively high-purity carbon dioxide, shown in result Fig. 1 of investigation.
Metal ion-modified phosphorus aluminium molecule of the skeleton sieve in table 1 and following all embodiment, all taking phosphorus aluminium molecule of the skeleton sieve SAPO-5 as carrier to load metal ion, but the phosphorus aluminium molecule of the skeleton of other type sieve can be used as equally carrier of the present invention and carrys out loaded metal ion, has equally very high adsorption efficiency.
Table 1
As known in table 1 data, the adsorption effect of the modification phosphorus aluminium molecule of the skeleton sieve of load five metal ion species obviously improves, wherein absorption property the best of the phosphorus aluminium molecule of the skeleton of loaded metal iron ion modification sieve.
Secondly, the charge capacity (massfraction) to loaded metal iron ion is investigated, and has investigated the impact of metallic iron ion load amount on this sorbent material absorption property, and the charge capacity of metallic iron ion and adsorption effect data are as shown in table 2.
Table 2
As known in table 2 data, when the charge capacity of metallic iron ion is 9% (massfraction), product sample purity can reach 99.990%, and absorption property is best.
Embodiment
Embodiment 1: the solution that iron nitrate is made into 1M, ratio with mass ratio 10:1 (catalyst raw powder: ammonium chloride) fully stirs it 3h at 60 DEG C, after stirring finishes, by mixture Büchner funnel suction filtration, with after deionized water wash, put into 110 DEG C, baking oven and dry 6h, be warming up to 550 at retort furnace Program, DEG C roasting 6h, repeats above-mentioned steps 2~3 times, has both obtained the phosphorus aluminium molecule of the skeleton sieve of metallic iron ion modification.
Then sieve as the sorbent material of preparing high-purity carbon dioxide using the phosphorus aluminium molecule of the skeleton of metallic iron ion modification, sorbent material is excessive, under the adsorption conditions of 25 DEG C of temperature of reaction, pressure 3.5MPa, air speed 80min-1, make the carbonic acid gas passing through remove sulfide if carbonyl sulfide (COS), hydrogen sulfide (H2S), oxidation products are as acetaldehyde, and hydrocarbon compound is as benzene, the purity of product can be to 99.999%.
Embodiment 2,3 and 4 is according to the step of embodiment 1, after the phosphorus aluminium molecule of the skeleton sieve of synthetic metallic iron ion modification, using it as the sorbent material of preparing high-purity carbon dioxide, under the adsorption conditions of pressure 3.5MPa and air speed 80min-1, different temperature of reaction in adsorption process, and sample purity data are as shown in table 3.
Table 3
As known in table 3 data, in embodiment 1,2,3 and 4, when temperature of reaction is 25 DEG C, the purity of product sample is 99.999%, is maximum in four embodiment, so select the temperature of reaction that 25 DEG C is adsorption process.
Embodiment 5,6,7 and 8 is according to the step of embodiment 1, after the phosphorus aluminium molecule of the skeleton sieve of synthetic metallic iron ion modification, using it as the sorbent material of preparing high-purity carbon dioxide, under the adsorption conditions of 25 DEG C of temperature of reaction and air speed 80min-1, different reaction pressure in adsorption process, and product sample purity data are as shown in table 4.
Table 4
As known in table 4 data, in embodiment 5,6,7 and 8, when reaction pressure is 3.5MPa and 4.5MPa, the purity of product sample all reaches 99.999%, but consider the pressure that bears of conversion unit, and work-ing life, the reaction pressure that 3.5MPa is adsorption process selected.
Embodiment 9,10,11,12 and 13 is according to the step of embodiment 1, after the phosphorus aluminium molecule of the skeleton sieve of synthetic metallic iron ion modification, using it as the sorbent material of preparing high-purity carbon dioxide, under the adsorption conditions of 25 DEG C of temperature of reaction and reaction pressure 3.5MP, air speed value in adsorption process, and product sample purity data are as shown in Figure 2.80min data are the result of embodiment 9, and 100min data are the result of embodiment 10, and 120min is the result of implementation data 11, and 140min data are the result of embodiment 12, and 160min is the result of embodiment 13.
As known in Fig. 2 data, in 80-160min, along with the increase of time, product sample purity constantly declines, and in the time of 80min, purity maximum, selects the air speed value of 80min as adsorption process.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the embodiment describing.

Claims (8)

1. a method of preparing high-purity carbon dioxide, is characterized in that, comprising:
Sieve as sorbent material taking metal ion-modified phosphorus aluminium molecule of the skeleton, the impurity in feed carbon dioxide is removed in absorption, and to obtain high-purity carbon dioxide, wherein, described metal ion is the one being selected from IB, IIIB and VIII family element.
2. the method for preparing high-purity carbon dioxide as claimed in claim 1, is characterized in that, described metal ion is nickel, copper, iron, cerium or silver element.
3. the method for preparing high-purity carbon dioxide as claimed in claim 2, is characterized in that, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of metal ion is 3%.
4. the method for preparing high-purity carbon dioxide as claimed in claim 1, is characterized in that, described metal ion is ferro element.
5. the method for preparing high-purity carbon dioxide as claimed in claim 4, is characterized in that, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of ferro element is 9%.
6. the method for preparing high-purity carbon dioxide as claimed in claim 5, is characterized in that, adsorption conditions is: 25 DEG C of temperature, pressure 3.5MPa, air speed 80min -1.
7. the method for preparing high-purity carbon dioxide as claimed in claim 1, is characterized in that, the particle diameter of described metal ion-modified phosphorus aluminium molecule of the skeleton sieve is 60~80 μ m.
8. the method for preparing high-purity carbon dioxide as claimed in claim 1, it is characterized in that, adopt equi-volume impregnating to prepare described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, wherein, the metal ion aqueous solution taking mass concentration as 3~15% is as steeping fluid, and dipping time is 10~100min.
CN201410265632.0A 2014-06-13 2014-06-13 A kind of method preparing high-purity carbon dioxide Expired - Fee Related CN104058402B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4440871A (en) * 1982-07-26 1984-04-03 Union Carbide Corporation Crystalline silicoaluminophosphates
CN1980725A (en) * 2004-03-19 2007-06-13 科罗拉多州立大学董事会 High-selectivity supported SAPO membranes

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4440871A (en) * 1982-07-26 1984-04-03 Union Carbide Corporation Crystalline silicoaluminophosphates
CN1980725A (en) * 2004-03-19 2007-06-13 科罗拉多州立大学董事会 High-selectivity supported SAPO membranes

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