CN113195408A - Production of sodium bicarbonate from carbon dioxide - Google Patents

Production of sodium bicarbonate from carbon dioxide Download PDF

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CN113195408A
CN113195408A CN202080007076.0A CN202080007076A CN113195408A CN 113195408 A CN113195408 A CN 113195408A CN 202080007076 A CN202080007076 A CN 202080007076A CN 113195408 A CN113195408 A CN 113195408A
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carbon dioxide
sodium bicarbonate
sodium
solution
ammonia solution
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帕维尼·辛塔拉科
查瓦特·泰查克里提卡尔
巴沃伦彭·简桑
汉查纳·盖特马拉
贡纳帕特·帕多温潘亚森
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00Carbonates of sodium, potassium or alkali metals in general
    • C01D7/18Preparation by the ammonia-soda process
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00Carbonates of sodium, potassium or alkali metals in general
    • C01D7/07Preparation from the hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

From carbon dioxide (CO)2) The preparation of sodium bicarbonate comprises the following steps: dissolving a sodium compound in deionized water to prepare a sodium compound solution; dissolving ammonia in deionized water to prepare an ammonia solution; mixing together a sodium compound solution and an ammonia solution under temperature controlled conditions and releasing carbon dioxide into the mixture to obtain a sodium bicarbonate product having the nature of a white solid; filtering the product from the solution and washing with an organic solvent; the product was then allowed to dry at room temperature.

Description

Production of sodium bicarbonate from carbon dioxide
Technical Field
The invention relates to the field of chemistry and chemical engineering science, and relates to the preparation of sodium bicarbonate from carbon dioxide.
Background
Global warming is a current global problem, adversely affecting humans, animals and the environment. The problem is mainly caused by greenhouse gases, especially carbon dioxide (CO)2) And wherein the carbon dioxide is produced by human activities such as waste incineration, cooking and agriculture. However, carbon dioxide produced during industrial processing is a major cause of greenhouse gas production.
To reduce carbon dioxide (CO)2) And to increase the value of carbon dioxide, a method has been developed to make full use of carbon dioxide, for example using carbon dioxide (CO)2) Carbon dioxide (CO) as a foaming agent in the dietary industry, such as in the production of soft drinks2) Conversion to agricultural urea, and use of carbon dioxide (CO)2) Chemicals are produced as reactants that can be used as raw materials in the petrochemical industry.
Sodium bicarbonate (NaHCO)3) Or the baking powder has white powder properties. It is mainly present in rock layers in the subsurface and is considered a natural mineral. It has been used in the food industry, animal feed industry, medical industry and cleaning industry. Now, sodium bicarbonate (NaHCO)3) Or baking powder can be made from sodium ions (Na) by the Solvay method known to those skilled in the art+) And carbon dioxide (CO)2) The method was discovered in 1861 by the chemical industry Ernest Solvay, Belgium.
According to the patent database, there is some prior art regarding the preparation of sodium bicarbonate, as shown in the examples below.
U.S. patent application publication No. US2622004A entitled "Cyclic Process for production of sodium bicarbonates and ammonium chloride" describes the synthesis of sodium bicarbonate (NaHCO) by the following method3): by this method, ammonia, water, sodium chloride (NaCl) and carbon dioxide (CO) are used at a preferred reaction temperature of 28 ℃ to 60 ℃2) As a reactant). The process always produces, for example, ammonium chloride (NH)4Cl) by-products.
Publication number WO2012050437A3 entitled "international patent application of Production of sodium bicarbonate from a basic process stream-a stream of gas flow containing a carbon dioxide organic from a burning at least one organic waste-treating a carbon dioxide-containing gas stream obtained from burning at least one organic waste or feed stream, on the one hand to product of the gas flow using an alkali carbonate water liquid on the one hand to produce sodium bicarbonate-quenching the gas stream using an alkali aqueous liquid"; european patent application with publication number EP1858807A1 entitled "Method for solidifying sodium carbonate crystals"; korean patent No. KR10157125 IB I; U.S. patent application publication No. US4405592A entitled "Process for producing anhydrous sodium carbonate crystals"; and U.S. patent application publication No. US3751560A entitled Multi-stage Process for the preparation of sodium bicarbonates describes sodium hydroxide (NaOH) and carbon dioxide (CO-A Multi-stage process for the preparation of sodium bicarbonate)2) Preparation of sodium bicarbonate (NaHCO) by reaction between3) Or baking powder.
In addition, the catalyst is prepared from sodium carbonate (NaCO)3) Water and carbon dioxide (CO)2) Reaction between the reactants of (a) to (b) to prepare sodium bicarbonate (NaHCO)3) Or baking powder as disclosed in 8th academic conference of Trondheim Conference on Capture,Transport and StEnergy Procedia 86(2016)47-55 (proceedings of Energy proceedings 86(2016) in orage (8 th conference on Telongham science for capture, transport and storage) entitled "CO" in the title of "Procedia 86(2016) (pages 47 to 55, proceedings of Energy science)")2capture and re-use at a waste incinerator (CO at waste incinerator)2Capture and reuse) "in international journal.
The above background of the present invention clearly shows that sodium ion (Na)+) And carbon dioxide (CO)2) Preparation of sodium bicarbonate (NaHCO) by reaction between3) Or the development of baking powder, which has been continuously developed from the past to the present. The invention discloses the use of carbon dioxide (CO)2) Sodium carbonate (Na)2CO3) (also known as soda ash or washing soda) and ammonia solution as reactants, at atmospheric pressure and at reaction temperatures below 60 ℃, sodium bicarbonate (NaHCO) is prepared without by-products3) Or baking powder.
Disclosure of Invention
The invention relates to the synthesis of carbon dioxide (CO)2) The preparation of sodium bicarbonate comprises the following steps: dissolving a sodium compound in deionized water to prepare a sodium compound solution; dissolving ammonia in deionized water to prepare an ammonia solution; mixing together a sodium compound solution and an ammonia solution under temperature controlled conditions and releasing carbon dioxide into the mixture to obtain a sodium bicarbonate product having the nature of a white solid; filtering the product from the solution and washing with an organic solvent; the product was then allowed to dry at room temperature.
The object of the present invention is to prepare sodium bicarbonate from carbon dioxide in a simple and highly safe process which yields highly purified sodium bicarbonate without by-products under atmospheric pressure conditions and at reaction temperatures below 60 ℃. The invention is suitable for industrial manufacturing and other industries, reduces the emission of carbon dioxide in the process of separating natural gas and improves the value of the carbon dioxide.
Drawings
FIG. 1 shows sodium bicarbonate (NaHCO) which can be produced in reactive ammonia solutions of different concentrations when using the process according to the invention3) X-ray diffraction pattern of (a).
FIG. 2 shows sodium bicarbonate (NaHCO) that can be produced when using the method according to the invention3) The percentage of (c) was compared with the reaction time at an operating pressure of 1 bar and 1.3 bar.
FIG. 3 shows sodium bicarbonate (NaHCO) that can be produced when using the method according to the invention3) The relationship between the percentage of (d) and the operating pressure compares the conditions at operating pressures of 1 bar to 5 bar.
Detailed Description
The invention relates to the synthesis of carbon dioxide (CO)2) Preparation of sodium bicarbonate (NaHCO)3). The method begins by mixing a sodium compound solution and an ammonia solution; then carbon dioxide (CO) is caused2) A reaction with a mixture of a sodium compound and an ammonia solution; and isolating the solid product of sodium bicarbonate produced. The preparation process comprises the following steps:
A. weighing a specified amount of a sodium compound selected from sodium carbonate (Na) and dissolving it in deionized water2CO3) Or sodium hydroxide (NaOH) or a combination thereof. The sodium compound is prepared at a temperature of between 20 ℃ and 60 ℃.
B. The indicated amount of ammonia was weighed and dissolved in deionized water. The preparation temperature of the ammonia solution is between 20 ℃ and 60 ℃.
C. The materials obtained from a. and b. are mixed together until the desired final concentrations of sodium compound and ammonia are obtained. Preferably, the final concentration of the mixed solution is: the sodium compound is between 1 mol/liter and 10 mol/liter and the ammonia solution is between 1 mol/liter and 5 mol/liter.
D. Mixing carbon dioxide (CO)2) Continuously released into the mixture obtained from c to cause the reaction at appropriate duration, temperature and pressure until a white solid product is produced. Preferably, carbon dioxide (CO) is used as a reactant2) Is between 99.5 volume percent and 99.9 volume percent.
Carbon dioxide (CO) to be used as a reactant2) Introducing a mixed solution of a sodium compound and an ammonia solution at a rate of 0.1 to 0.5 literMin/0.2 liter total liquid volume; the operating pressure is between 1 bar and 5 bar; preferably at a temperature between 20 ℃ and 60 ℃; and carbon dioxide (CO)2) The preferred duration of the passage into the mixed solution of the sodium compound and the ammonia solution is between 1 hour and 10 hours.
E. The white solid product obtained from d. is filtered from the solution by a method such as filter paper until it is dried and washed again with an organic solvent. The product was allowed to dry at room temperature for 5 to 10 days and then weighed, where it was washed with carbon dioxide (CO)2) The organic solvent of the white solid product obtained by the reaction with the mixed solution of the sodium compound and the ammonia solution is an alcohol-based organic solvent, preferably ethanol. Sodium bicarbonate was then tested for identity by comparing it to sodium bicarbonate standards using X-ray diffraction (XRD) analysis techniques to analyze its purity and crystal structure.
The product obtained from the chemical reaction was calculated as percent yield based on the following formula:
percent yield 100 actual/theoretical yield
Where the actual yield is the amount of product obtained from the test or reaction and the theoretical yield is the amount of product obtained from the chemical equation for a complete reaction.
Since the sodium bicarbonate product can be partially dissolved in water, the percent yield is less than 100%. The solubility of sodium bicarbonate at 20 ℃ was found to be 96 grams per 1 liter of water, and the reaction was also found to be incomplete under the conditions tested.
One or more embodiments of the present invention will be described in detail with reference to examples of the preparation of a sodium bicarbonate solid product according to the present invention. However, there is no intention to limit one or more embodiments of the invention. The following examples are provided to illustrate certain embodiments in terms of their functionality. It will be clearly understood by those skilled in the art that the present invention is not limited to certain embodiments illustrated in these examples.
Example 1
This example describes the preparation of a polycarbonate by carbonation at atmospheric pressureSodium (Na)2CO3) Ammonia solution and carbon dioxide (CO)2) The process for the preparation of solid sodium bicarbonate product and also the results of the concentration of the ammonia solution used as reactant for each amount of solid sodium bicarbonate product prepared, as follows:
weighing sodium carbonate (Na)2CO3)63.6 grams, was dissolved in deionized water and an ammonia solution was prepared at a concentration of 0 to 3.72 moles/liter free of deionized water.
The prepared sodium carbonate solution and ammonia solution were mixed together until the final mixed solution volume was 200 ml, and the final concentrations of the mixed solutions of the sodium carbonate solution and ammonia solution were 3 mol/l and 2.66 mol/l, respectively. Then, carbon dioxide having a concentration of 99.9 volume percent was released into the mixed solution in the open container at a flow rate of 200 ml/min to allow reaction at a temperature of 25 ℃ and atmospheric pressure for 5 hours until a white solid product was produced.
The white solid product was filtered from the solution through No. 1 filter paper until it was dried and washed again with ethanol organic solvent. The product was then allowed to dry at room temperature for 5 to 10 days to eliminate the water.
The white solid product obtained was weighed for calculating the percent yield. The results are shown in table 1. The white solid product was then taken and tested for sodium bicarbonate identity by comparison with sodium bicarbonate standards and commercial sodium bicarbonate products using X-ray diffraction analysis techniques.
Table 1 results of the concentration of ammonia solution used as a reactant for each percent yield
Figure BDA0003119458300000051
According to table 1, it was found that increasing the concentration of the ammonia solution used as a reactant significantly contributes to the increase in percent yield, and an appropriate concentration of ammonia solution of 2.66 moles/liter can increase the percent yield of the sodium bicarbonate solid product from 21.85% to 38.13% in the system without the ammonia solution.
Furthermore, increasing the concentration of the ammonia solution used as a reactant does not affect the product purity, since no strange peaks are found in the synthesized samples when the obtained sodium bicarbonate solid product is analyzed using X-ray diffraction analysis techniques. However, the peak intensity of the synthesized sodium bicarbonate sample does not correspond to the sodium bicarbonate standard, since the obtained product has different crystalline properties, as shown in fig. 1.
Example 2
The preparation process is similar to that of example 1, except that carbon dioxide (CO) is used2) The duration of the passage of the mixed solution of the sodium compound and the ammonia solution was between 1 hour and 10 hours, providing the test results shown in table 2.
Table 2 carbon dioxide (CO) per percent yield of sodium bicarbonate product produced2) Duration results of the passage into the mixture of sodium carbonate solution and ammonia solution
Figure BDA0003119458300000061
According to table 2, it was found that increasing the reaction duration significantly increased the percentage yield of the sodium bicarbonate solid product, and that only a small change in the percentage yield after 5 hours indicated by carbon dioxide (CO)2) A suitable reaction duration for the synthesis of sodium bicarbonate is 5 hours.
Example 3
The preparation method was similar to that of example 1 except that sodium hydroxide (NaOH) was used as a reactant, wherein the final concentration of sodium ions in the mixed solution was 6 moles/liter before the carbon dioxide was introduced. The results of the concentration of the ammonia solution used as reactant for each volume of solid product of sodium bicarbonate produced are also described, as shown in table 3.
Table 3 results of the concentration of ammonia used as a reactant for the yield per percent of solid sodium bicarbonate product produced when using sodium hydroxide as a reactant
Concentration of reactive Ammonia solution (mol/l) Percent yield
0 0.5
1.59 30.1
According to table 3, it was found that the percentage yield of sodium bicarbonate produced was significantly increased when ammonia was present in the system.
Example 4
The preparation method was similar to that of example 1 except that the final concentration of ammonia in the mixed solution before the carbon dioxide gas was introduced was 1.59 mol/l. In addition, a comparison was made using sodium hydroxide (NaOH) and sodium chloride (NaCl) as reactive sodium compounds, with final sodium ion concentrations of 6 moles/liter and 1.59 moles/liter, respectively, prior to the introduction of carbon dioxide and ammonia into the mixture, providing the test results shown in table 4.
Table 4 results at final concentrations of each type of reactive sodium compound for each percent yield of sodium bicarbonate produced prior to carbon dioxide injection, where the final concentrations of the sodium ion and ammonia solutions in the mixed solution were 6 moles/liter and 1.59 moles/liter
Type of reactive sodium compound Percent yield
Sodium carbonate (Na)2CO3) Example 1 34.74
Sodium hydroxide (NaOH) 30.1
Sodium chloride (NaCl) 18.2
From the test results, it was found that the type of reactive sodium compound affected the percent yield of sodium bicarbonate produced. Further, when sodium chloride (NaCl) is used as the reactive sodium compound, according to the solvay method, such as ammonium chloride (NH) always appears4Cl) by-products.
Example 4
The preparation process was similar to that of example 2, except that the operating pressure in the pressure-controlled vessel was 1.3 bar, and the test results are shown in fig. 2, which indicates that the percent yield of sodium bicarbonate prepared increases as the operating pressure increases.
Example 5
The preparation process was similar to that of example 1, except that the pressure in the pressure-controlled vessel was 1 bar to 5 bar, and the test results are shown in fig. 2, which shows that the percent yield of sodium bicarbonate prepared increases when the operating pressure is significantly increased from 1 bar to 3 bar, and that the percent yield changes only slightly after the operating pressure is greater than 3 bar.
Of the many possible embodiments in which the principles of the disclosed invention may be employed, the disclosed embodiments are merely preferred examples of the invention and should not be taken to limit the scope of the invention.
The following defined additional description of the terms and methods is provided to better describe the present disclosure and to suggest themselves to those skilled in the art for putting this disclosure into practice.
Unless otherwise indicated, the total amount of components, molecular weights, percentages, temperatures, times, and the like as recited in the specification or claims may even be understood as modified by the word "about," unless otherwise expressly indicated or implied. Those numerical variables mentioned are estimates of the properties and/or inspection limits that may be expected to be achieved under standard test conditions/methods, which estimates may be understood by those skilled in the art when directly or explicitly distinguishing embodiments from previously described embodiments.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. Although similar or equivalent methods and materials described herein can be used in the practice or testing of the present disclosure, the preferred methods and material samples are further described. The methods, materials, and samples are illustrative of certain embodiments or are not intended to be limiting.
It will be apparent to those skilled in the art that certain compounds may be further described in combination with the definitions of terms such as, for example, group 7 of the periodic table of elements referred to by those skilled in the art as halogen.
Certain atoms in the structure, such as carbon, hydrogen, or hydrogen atoms, are sometimes indicated by characters. For example, -CH2CH2It will be appreciated by those skilled in the art that this is a common technique in the chemical arts for shortening and simplifying the description of organic chemistry.
Functional groups are a specific set of atoms within a molecule that are responsible for the characteristic chemical reactions of these molecules. Examples of functional groups include, but are not limited to, alkanes, alkenes, alkynes, halides (fluorine, chlorine, bromine, iodine), hydroxyls (OH), carbonyls (ketones), aldehydes (HCOR), esters (COOR), and Carboxylates (COO)-)。
Alcohols are organic compounds comprising at least one hydroxyl group. It may be a monohydric alcohol containing one-OH group, a dihydric or dihydric alcohol containing two-OH groups such as ethylene glycol, a trihydric or trihydric alcohol containing three-OH groups such as glycerol, a polyhydric alcohol containing three or more-OH groups.
Best mode for carrying out the invention
The best mode of the present invention is as described in the detailed description of the present invention.

Claims (10)

1. The preparation of sodium bicarbonate from carbon dioxide comprises the following steps:
a. weighing a specified amount of a sodium compound and dissolving the sodium compound in deionized water to prepare a sodium compound solution;
b. weighing a specified amount of ammonia and dissolving it in deionized water to prepare an ammonia solution;
c. mixing together the solutions obtained from a. The sodium compound is between 1 mol/liter and 10 mol/liter and the ammonia solution is between 1 mol/liter and 5 mol/liter;
d. releasing carbon dioxide into the mixture obtained from c. under controlled flow rate, time, temperature and pressure conditions, resulting in a sodium bicarbonate product having white solid properties;
e. the product obtained from d. was filtered from the solution and allowed to dry at room temperature.
2. Sodium bicarbonate from carbon dioxide according to claim 1 wherein the sodium compound is selected from sodium carbonate or sodium hydroxide or a combination thereof.
3. Sodium bicarbonate prepared from carbon dioxide according to claims 1 to 2, wherein the concentration of carbon dioxide is comprised between 99.5 and 99.9 volume%.
4. Sodium bicarbonate from carbon dioxide according to claims 1 to 3, wherein the rate of carbon dioxide passage into the mixed solution of sodium compound and ammonia solution is comprised between 0.1 and 0.5 liters/min/0.2 liters of total liquid.
5. Sodium bicarbonate from carbon dioxide according to claims 1 to 4, wherein the preferred duration of the passage of carbon dioxide into the mixed solution of sodium compound and ammonia solution is comprised between 1 and 10 hours.
6. Sodium bicarbonate from carbon dioxide according to claims 1 to 5 wherein the preferred temperature during the preparation of the sodium compound, the ammonia solution or the passage of carbon dioxide into the mixed solution of sodium compound and ammonia solution is comprised between 20 ℃ and 60 ℃.
7. Sodium bicarbonate from carbon dioxide according to claims 1 to 6, wherein the preferred pressure during the passage of carbon dioxide into the mixed solution of sodium compound and ammonia solution is comprised between 1 bar and 5 bar.
8. Sodium bicarbonate preparation from carbon dioxide according to claims 1 to 7 wherein the filtration of the sodium bicarbonate product from the solution additionally comprises washing the product with an organic solvent after said filtration.
9. Sodium bicarbonate prepared from carbon dioxide according to claims 1 to 8, wherein the organic solvent is an alcoholic organic solvent.
10. Sodium bicarbonate preparation from carbon dioxide according to claims 1 to 9 wherein the alcoholic organic solvent is ethanol.
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US5275794A (en) * 1991-11-20 1994-01-04 Luna Raymundo R Process for producing sodium bicarbonate from natural soda salts
US5288472A (en) * 1993-02-08 1994-02-22 Ruiz Raymundo L Process for the recovery of the sodium hydroxide and sodium chloride from the effluent of a diaphragm cell as solid sodium bicarbonate
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CN108147435A (en) * 2018-02-05 2018-06-12 重庆宜化化工有限公司 A kind of carbonization technique for soda manufacture

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