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WO2010140989A1 - Production de carbonate de bore et de bicarbonate de sodium à partir de solvants de borate de sodium - Google Patents

Production de carbonate de bore et de bicarbonate de sodium à partir de solvants de borate de sodium Download PDF

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Publication number
WO2010140989A1
WO2010140989A1 PCT/TR2009/000110 TR2009000110W WO2010140989A1 WO 2010140989 A1 WO2010140989 A1 WO 2010140989A1 TR 2009000110 W TR2009000110 W TR 2009000110W WO 2010140989 A1 WO2010140989 A1 WO 2010140989A1
Authority
WO
WIPO (PCT)
Prior art keywords
sodium
carbonate
boric
gas
range
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/TR2009/000110
Other languages
English (en)
Inventor
Orhan Yilmaz
Fehmi Unlu
Goknur Karakoc
Derya Maraslioglu
Soner Gokcek
Ebru Karacay
M. Hamdi Demirhan
C. Emrah Cetin
Omer Iplikcioglu
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ETI MADEN ISLETMELERI GENEL MUDURLUGU
Original Assignee
ETI MADEN ISLETMELERI GENEL MUDURLUGU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ETI MADEN ISLETMELERI GENEL MUDURLUGU filed Critical ETI MADEN ISLETMELERI GENEL MUDURLUGU
Publication of WO2010140989A1 publication Critical patent/WO2010140989A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D13/00—Compounds of sodium or potassium not provided for elsewhere
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00—Carbonates of sodium, potassium or alkali metals in general
    • C01D7/07—Preparation from the hydroxides

Definitions

  • the invention relates to a new product (boric carbonate) obtained by means of passing CO 2 (carbon dioxide) gas through the diluted solvents of sodium borate produced from all-in concentrated and calcined tincal by use of autoclave (1) (high pressured and temperature reactor) jacket reactors (4) and gas absorption column (7) systems and also to obtaining pure sodium bicarbonate as a result of extraction of the said product by methyl alcohol.
  • a new product (boric carbonate) obtained by means of passing CO 2 (carbon dioxide) gas through the diluted solvents of sodium borate produced from all-in concentrated and calcined tincal by use of autoclave (1) (high pressured and temperature reactor) jacket reactors (4) and gas absorption column (7) systems and also to obtaining pure sodium bicarbonate as a result of extraction of the said product by methyl alcohol.
  • Borax decahydrate Na 2 B 4 O 7 -IOH 2 O
  • Borax pentahydrate Na 2 B 4 O 7 .5H 2 O
  • Borax pentahydrate is a sodium borate hydrate of trigonal structure with 1,880 g/cm 3 density.
  • Commercial borax pentahydrate generally contains 4,67 mol water.
  • borax increases with increase in temperature and solubility curves of penta and deca- hydrates intersect at about 60,6 0 C and 60,8 0 C . From here, it is understood that in case the saturated borax at 100 0 C is cooled to 60 0 C, borax pentahydrate is crystallized and in case of repeating the same process at lower temperatures, borax decahydrate is crystallized.
  • the second raw material used in the study is CO 2 gas, which has been felt much more recently and one of the most important greenhouse gas causing global warming, It is a gas having a rich and wide range of use in several industries due to its multi purposed features and capable to dissolve in water and indicating acidic feature.
  • Other physical features of the CO 2 gas has been given below and it is heavier than air; is odorless and colorless, may convert into solid form at atmospheric pressure and is in liquid form under pressure. It does not support flaming.
  • NaHCO 3 and B 2 O 3 production is in a reactor convenient for mixing with heated jacket by applying the room temperature between 175 - 200 0 C, preferably 200 0 C, CO 2 pressure between 10 - 750 psi [0.68 - 51 atm] preferably 30 - 40 atm .
  • FIG. 1 Boric carbonate production in Jacket Reactor (4) system
  • Figure 3 Boric carbonate production in Gas Absorption Column system
  • Sodium carbonate and boron containing new products are obtained from reaction of water solutions prepared from sodium borates with CO 2 gas. These products are used as new products depending on their consumption area and can also be classified as sodium carbonates and borates. Different systems have been used in realization of the reaction and the formation parameters of the product according to the systems have been specified.
  • Sodium borates of 0.44 and 0.88 molar Na 2 0/B 2 0 3 rate with weight 3,5% - 2I Na 2 O content solvents were prepared and sodium borate products of sodium bicarbonate content of 2 - 80 % and 5 - 44% B 2 O 3 were obtained during reaction time of 60-420 minutes, preferably subjecting to the reaction for 120 minutes, 20-800 psi range CO 2 gas pressure, 550 cycle/minute mixing rate and , preferably 12,7% Na 2 O content,, temperature of 20- 75 0 C preferably 60 0 C 1 .
  • the carbonate and boron amounts as per the product intended to be obtained depending on area of use can be obtained at the study conditions given in Table 1.
  • Table 1 shows the summary of the conducted studies.
  • Sodium borate solutions to be prepared as per the final product intended to be obtained of % Na 2 O by weight are subjected to reaction at the above mentioned temperature, pressure and the duration in the autoclave (1) device.
  • the sludgy article obtained after the reaction time is sent to the filter (2) unit designed according to pressure filtration principle by help of a hose installed at the drainage valve of the autoclave (1) device at 52 - 54 0C and the product filtered at operating pressure is then subjected to filtration with vacuum at the filter (2) unit by applying pressure with CO 2 gas again.
  • the cake contains 7% humidity and is dried in drying oven (3) at 30 - 40 0 C.
  • the boric carbonate product obtained in this way also contains sodium borate not entering in the reaction.
  • the system is intermittent the obtained solution can be used as feed again and therefore provides recycling process.
  • sodium borate and NaB 5 O 6 (OH) 4 (H 2 O) 3 (sborgite) mixture not entered into reaction is obtained as a side product.
  • Process flow chart for the studies conducted at jacket reactor (4) is given in Figure 2.
  • CO 2 gas is fed into the solutions of sodium borate containing 0,44 and 0,88 molar prepared in concentrations of 4,6 - 4,8% Na 2 O by weight, by means of a line (5) installed into the jacket reactor (4).
  • Reaction temperature is adjusted by cryostat (6) connected to the jacket reactor (4).
  • the crystals obtained from the sodium borate solution prepared with 4,6 - 4,8 % Na 2 O by weight in the study conducted at 50 - 60 C temperature, 12 hours reaction time, under atmospheric pressure and 500 cycles/minute mixing rate are subjected to filtration by vacuuming by filter (2) at -5 - 50 C and dried at drying oven (3) at 30-40 C.
  • the obtained product is sodium bicarbonate of 5-12% and sodium borate of B 2 O 3 of 32 -37%.
  • the boric carbonate product obtained in this way also contains sodium borate not entering in the reaction.
  • sodium borate and NaB 5 O 6 (OH) 4 (H 2 O) 3 (sborgite) mixture not entered into reaction is obtained as a side product.
  • Table 2 The summary of the studies have been shown in Table 2.
  • Saturated sodium borate solution containing 0,44 and 0,88 Na 2 0/B 2 O 3 mol of pH > 9 prepared according to working temperature is located in the feeding tank (8) of the filled gas absorption column (7).
  • the solution in the feeding tank (8) is heated to 45-70 0 C, preferably 60 C by means of heater (9).
  • the solution is sent to the upper part of the gas absorption column (7) (from the solution tank at the feeding rate of 400 ml/minute - 1500 ml/minute, preferably 1000 ml/minute by means of peristaltic pump, and flows downward from column over filling surface and absorbs CO 2 gas. Recycling of the solution from lower part is provided.
  • 0,5 - 1 bar CO 2 gas and air mixture is sent upward in reverse direction from lower part of the absorption column (7).
  • This cycling is continued for 240-480 minutes by adding sodium borate solution to the system in order to ensure pH >8 .
  • the solution obtained at the end of the reaction duration is transmitted to jacket reactor (4) and subjected to crystallization at temperature range of 5 - 50 0 C.
  • the crystals formed in the solution are vacuumed at filter (2) unit " and subjected to filtration.
  • the obtained product crystals is dried at drying oven (6) at temperature range of 30 - 40 °C.
  • boric carbonate content consists of sodium borate of 30 - 37% B 2 O 3 value and sodium bicarbonate of 3-25%.
  • the boric carbonate product obtained from autoclave (1), jacket reactor (4) and gas absorption column (7) systems is pure carbonate obtained by extraction process by use of dissolution of the products in different solvents.
  • the feature of borate to dissolve in methyl alcohol has been used for extraction process. To achieve it, 5% more methyl alcohol than the dissolution value of borate in methyl alcohol in the product at 30 0 C has been added and mixing has been applied for 1 hour and the obtained solvent has been subjected to filtration. The cake obtained as a result of the filtration is 98-99% sodium bicarbonate with 87% efficiency.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

L'invention a pour objet l'obtention d'une nouvelle solution saline de sodium constituée de carbonate et de bore, pour assurer une facilité d'utilisation dans des secteurs industriels à l'aide de carbonate de sodium et de borate de sodium et également l'utilisation, en tant que matière première, du gaz CO2 qui constitue le gaz à effet de serre aux conséquences les plus importantes parmi celles ressenties le plus récemment et entraînant un réchauffement mondial et ainsi réduire l'émission de gaz CO2 dans l'environnement. L'invention concerne un nouveau produit (carbonate de bore) obtenu en faisant passer du gaz CO2 (dioxyde de carbone) dans les solvants dilués de borate de sodium à l'aide de systèmes d'autoclave (1), de réacteurs chemisés (réacteur à haute température et à haute pression) (4) et de colonne d'absorption de gaz (7), ainsi que l'obtention de carbonate pur comme résultat d'extraction dudit produit à l'aide d'alcool méthylique.
PCT/TR2009/000110 2009-06-05 2009-08-26 Production de carbonate de bore et de bicarbonate de sodium à partir de solvants de borate de sodium Ceased WO2010140989A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
TR2009/04415A TR200904415A2 (tr) 2009-06-05 2009-06-05 Sodyum borat çözelti̇leri̇nden co2 gazi geçi̇ri̇lmesi̇ i̇le sodyum borat ve sodyum bi̇karbonat karişim ürünü ve sodyum bi̇karbonat üreti̇mi̇
TR2009/04415 2009-06-05

Publications (1)

Publication Number Publication Date
WO2010140989A1 true WO2010140989A1 (fr) 2010-12-09

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/TR2009/000110 Ceased WO2010140989A1 (fr) 2009-06-05 2009-08-26 Production de carbonate de bore et de bicarbonate de sodium à partir de solvants de borate de sodium

Country Status (2)

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TR (1) TR200904415A2 (fr)
WO (1) WO2010140989A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105480986A (zh) * 2014-10-15 2016-04-13 刘浩 一种硼酸制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2884440A (en) 1956-04-10 1959-04-28 Olin Mathieson Preparation of borate esters
GB861416A (en) 1958-02-13 1961-02-22 United States Borax Chem Production of boric acid
US3031264A (en) 1958-02-13 1962-04-24 United States Borax Chem Production of boric acid
DE2139924A1 (de) * 1970-08-13 1972-02-17 Solvay Verfahren zur Gewinnung von Natrium bicarbonat, Borsaure und/oder Boroxyd
US4022871A (en) 1974-12-16 1977-05-10 Solvay & Cie Process for the fabrication of sodium bicarbonate and boric acid from borosodium ores
US20030003038A1 (en) * 2001-04-12 2003-01-02 Amendola Steven C. Processes for synthesizing borohydride compounds

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2884440A (en) 1956-04-10 1959-04-28 Olin Mathieson Preparation of borate esters
GB861416A (en) 1958-02-13 1961-02-22 United States Borax Chem Production of boric acid
US3031264A (en) 1958-02-13 1962-04-24 United States Borax Chem Production of boric acid
DE2139924A1 (de) * 1970-08-13 1972-02-17 Solvay Verfahren zur Gewinnung von Natrium bicarbonat, Borsaure und/oder Boroxyd
US4022871A (en) 1974-12-16 1977-05-10 Solvay & Cie Process for the fabrication of sodium bicarbonate and boric acid from borosodium ores
US20030003038A1 (en) * 2001-04-12 2003-01-02 Amendola Steven C. Processes for synthesizing borohydride compounds

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Production of Boric Acid and Sodium Bicarbonate from Sodium Tetraborate by means of carbonation", MASTER THESIS, HAYRETTIN YÜCEL MIDDLE EAST TECHNICAL UNIVERSITY, 1973

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105480986A (zh) * 2014-10-15 2016-04-13 刘浩 一种硼酸制备方法

Also Published As

Publication number Publication date
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