CN104058402B - A kind of method preparing high-purity carbon dioxide - Google Patents
A kind of method preparing high-purity carbon dioxide Download PDFInfo
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- CN104058402B CN104058402B CN201410265632.0A CN201410265632A CN104058402B CN 104058402 B CN104058402 B CN 104058402B CN 201410265632 A CN201410265632 A CN 201410265632A CN 104058402 B CN104058402 B CN 104058402B
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- carbon dioxide
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- purity carbon
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Abstract
The invention belongs to purifying technical field, be specifically related to a kind of method preparing high-purity carbon dioxide, is adopt how metal ion-modified phosphorus aluminium molecule of the skeleton sieve series for the processing method of high-purity carbon dioxide.The phosphorus aluminium molecule of the skeleton sieve of the first synthetic metals ion modification of the present invention, then with it for sorbent material, impurity in absorption removing feed carbon dioxide, and by investigating temperature of reaction, reaction pressure and the air speed value in adsorption process, obtain high-purity carbonic acid gas, the purity of finally prepd carbonic acid gas can reach 99.999%, Be very effective.The metal ion-modified phosphorus aluminium molecule of the skeleton sieve series that the present invention relates to uses less for high-purity carbon dioxide processing unit, floor space is little, save the energy, reduce costs, and is economizing on resources and is having great social benefit in the energy, environment protection etc.
Description
Technical field
The invention belongs to purifying technical field, be specifically related to a kind of method preparing high-purity carbon dioxide, is adopt how metal ion-modified phosphorus aluminium molecule of the skeleton sieve series for the processing method of 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, especially in industrial application etc., tool has been widely used, the application, supercritical extraction etc. of drink industry, so it is extremely important to prepare highly purified carbonic acid gas.Being applied to the mainly oxidation of carbon dioxide purification purification at present, absorption, there is use equipment many in distillation conventional steps of etc.ing, and floor space greatly, consumes energy high, and efficiency is low with high in cost of production problem.
Summary of the invention
The object of this invention is to provide a kind of method preparing high-purity carbon dioxide, is adopt how metal ion-modified phosphorus aluminium molecule of the skeleton sieve series for the processing method of high-purity carbon dioxide.Metal ion-modified phosphorus aluminium skeleton analysis is adopted to sieve synthesis carbonic acid gas; purity can reach 99.999%; the method makes several technological process be integrated; minimizing equipment, floor space and operator, the saving energy, to reduce costs; more effective than traditional thinking and countermeasure, economizing on resources and in the energy, environment protection etc., there is great social benefit.There is great scientific meaning and social application prospect.
The solution of the present invention is:
Prepare a method for high-purity carbon dioxide, comprising:
With metal ion-modified phosphorus aluminium molecule of the skeleton sieve for sorbent material, the impurity in absorption removing feed carbon dioxide, to obtain high-purity carbon dioxide, wherein, described metal ion is be selected from the one in IB, IIIB and VIII element.
Preferably, described prepares in the method for high-purity carbon dioxide, and described metal ion is nickel, copper, iron, cerium or silver element.
Preferably, described prepares in the method for high-purity carbon dioxide, and in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of metal ion is 3%.
Preferably, described prepares in the method for high-purity carbon dioxide, and described metal ion is ferro element.
Preferably, described prepares in the method for high-purity carbon dioxide, and in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of ferro element is 9%.
Preferably, described prepares in the method for high-purity carbon dioxide, and adsorption conditions is: temperature 25 DEG C, pressure 3.5MPa, air speed 80min
-1.
Preferably, described prepares in the method for high-purity carbon dioxide, and the particle diameter of described metal ion-modified phosphorus aluminium molecule of the skeleton sieve is 60 ~ 80 μm.
Preferably, described prepares in the method for high-purity carbon dioxide, adopts equi-volume impregnating to prepare described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, wherein, take mass concentration as the aqueous metallic ions of 3 ~ 15% be steeping fluid, 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.
Accompanying drawing explanation
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, can implement according to this with reference to specification sheets word to make those skilled in the art.
Prepare a method for high-purity carbon dioxide, comprising:
With metal ion-modified phosphorus aluminium molecule of the skeleton sieve for sorbent material, the impurity in absorption removing feed carbon dioxide, to obtain high-purity carbon dioxide, wherein, described metal ion is be selected from the one in IB, IIIB and VIII element.
Described prepares in the method for high-purity carbon dioxide, and described metal ion is nickel, copper, iron, cerium or silver element.
Described prepares in the method for high-purity carbon dioxide, and in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of metal ion is 3%.
Described prepares in the method for high-purity carbon dioxide, and described metal ion is ferro element.
Preferably, described prepares in the method for high-purity carbon dioxide, and in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of ferro element is 9%.
Described prepares in the method for high-purity carbon dioxide, and adsorption conditions is: temperature 25 DEG C, pressure 3.5MPa, air speed 80min
-1.
Described prepares in the method for high-purity carbon dioxide, and the particle diameter of described metal ion-modified phosphorus aluminium molecule of the skeleton sieve is 60 ~ 80 μm.
Described prepares in the method for high-purity carbon dioxide, and adopt equi-volume impregnating to prepare described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, wherein, take mass concentration as the aqueous metallic ions of 3 ~ 15% be steeping fluid, dipping time is 10 ~ 100min.
Prepare the nickelous nitrate of 1M, cupric nitrate, iron nitrate, cerous nitrate and Silver Nitrate steeping fluid respectively, the metal ions such as nickel, copper, iron, cerium and silver are made to 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 high-purity carbon dioxide respectively, shown in result Fig. 1 of investigation.
Metal ion-modified phosphorus aluminium molecule of the skeleton sieve in table 1 and following all embodiments, all for carrier to load metal ion with phosphorus aluminium molecule of the skeleton sieve SAPO-5, but the phosphorus aluminium molecule of the skeleton of other type sieve can carry out loaded metal ion as carrier of the present invention equally, has very high adsorption efficiency equally.
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 significantly improves, and the absorption property of the phosphorus aluminium molecule of the skeleton sieve of wherein loaded metal iron ion modification is best.
Secondly, investigate the charge capacity (massfraction) of loaded metal iron ion, investigated metallic iron ion load amount to the impact of this adsorbent performance, charge capacity and the adsorption effect data of metallic iron ion 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 samples purity can reach 99.990%, and absorption property is best.
Embodiment
Embodiment 1: solution iron nitrate being made into 1M, with the ratio of mass ratio 10:1 (catalyst raw powder: ammonium chloride), it is fully stirred 3h at 60 DEG C, after stirring terminates, mixture is used Büchner funnel suction filtration, after deionized water wash, put into 110 DEG C, baking oven and dry 6h, 550 are warming up 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 using the phosphorus aluminium molecule of the skeleton of metallic iron ion modification sieve as the sorbent material preparing high-purity carbon dioxide, sorbent material is excessive, under the adsorption conditions of temperature of reaction 25 DEG C, pressure 3.5MPa, air speed 80min-1, make the carbonic acid gas removing sulfide passed through if carbonyl sulfide (COS), hydrogen sulfide (H2S), oxidation products are as acetaldehyde, and hydrocarbon compound is as benzene, the purity of product can 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 metals iron ion modification, using it as the sorbent material 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 samples is 99.999%, is maximum in four embodiments, so selecting 25 DEG C is the temperature of reaction of 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 metals iron ion modification, using it as the sorbent material preparing high-purity carbon dioxide, under the adsorption conditions of temperature of reaction 25 DEG C with air speed 80min-1, different reaction pressure in adsorption process, and Product samples purity data is 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 samples all reaches 99.999%, but that considers conversion unit bears pressure, and work-ing life, 3.5MPa is selected to be the reaction pressure of adsorption process.
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 metals iron ion modification, using it as the sorbent material preparing high-purity carbon dioxide, under the adsorption conditions of temperature of reaction 25 DEG C with reaction pressure 3.5MP, air speed value in adsorption process, and Product samples purity data is 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 samples purity constantly declines, and when 80min, purity is maximum, selects 80min as the air speed value of adsorption process.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, 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 described.
Claims (4)
1. prepare a method for high-purity carbon dioxide, it is characterized in that, comprising:
With metal ion-modified phosphorus aluminium molecule of the skeleton sieve for sorbent material, the impurity in absorption removing feed carbon dioxide, to obtain high-purity carbon dioxide, wherein, adsorption conditions is: temperature 25 DEG C, pressure 3.5MPa, air speed 80min
-1, described metal ion is be selected from the one in copper, cerium or silver element.
2. prepare the method for high-purity carbon dioxide as claimed in claim 1, it is characterized in that, in described metal ion-modified phosphorus aluminium molecule of the skeleton sieve, the charge capacity of metal ion is 3%.
3. prepare the method for high-purity carbon dioxide as claimed in claim 1, it is characterized in that, the particle diameter of described metal ion-modified phosphorus aluminium molecule of the skeleton sieve is 60 ~ 80 μm.
4. prepare the method for 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, take mass concentration as the aqueous metallic ions of 3 ~ 15% be steeping fluid, dipping time is 10 ~ 100min.
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| CN104058402B true CN104058402B (en) | 2016-04-27 |
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Citations (2)
| 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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2014
- 2014-06-13 CN CN201410265632.0A patent/CN104058402B/en not_active Expired - Fee Related
Patent Citations (2)
| 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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