JPS6363485B2 - - Google Patents
Info
- Publication number
- JPS6363485B2 JPS6363485B2 JP11923281A JP11923281A JPS6363485B2 JP S6363485 B2 JPS6363485 B2 JP S6363485B2 JP 11923281 A JP11923281 A JP 11923281A JP 11923281 A JP11923281 A JP 11923281A JP S6363485 B2 JPS6363485 B2 JP S6363485B2
- Authority
- JP
- Japan
- Prior art keywords
- caustic soda
- anhydrous
- temperature
- aqueous solution
- cleaning
- 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.)
- Expired
Links
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 69
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 36
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 23
- 239000013078 crystal Substances 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 239000001569 carbon dioxide Substances 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 235000017550 sodium carbonate Nutrition 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 14
- 239000012535 impurity Substances 0.000 description 7
- 235000002639 sodium chloride Nutrition 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229940076133 sodium carbonate monohydrate Drugs 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 150000004682 monohydrates Chemical class 0.000 description 2
- 229940001593 sodium carbonate Drugs 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
【発明の詳細な説明】
本発明は、無水炭酸ソーダ結晶の洗浄方法に関
する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for cleaning anhydrous sodium carbonate crystals.
無水炭酸ソーダ結晶は各種の方法で製造される
が、結晶表面に付着した各種不純物あるいは溶液
を除去したい場合が多い。 Anhydrous sodium carbonate crystals are produced by various methods, but in many cases it is desired to remove various impurities or solutions attached to the crystal surface.
通常は水で洗浄し、乾燥することが考えられる
が、この方法では次のような欠点がある。 Normally, washing with water and drying is considered, but this method has the following drawbacks.
その１つは、水で洗浄することにより、無水炭
酸ソーダの表面が炭酸ソーダ含水塩（普通は１水
塩）に転移することである。 One is that by washing with water, the surface of anhydrous soda carbonate transforms into a hydrated salt of sodium carbonate (usually monohydrate).
他の１つは、無水炭酸ソーダ結晶の表面が溶解
流失し、無水炭酸ソーダ結晶の歩留が低下するこ
とである。 Another problem is that the surface of the anhydrous sodium carbonate crystals is dissolved and washed away, resulting in a decrease in the yield of the anhydrous soda carbonate crystals.
本発明者等は、上記欠点を克服する努力を重
ね、特定の条件下で苛性ソーダ水溶液で洗浄する
ことにより、この問題を解決することに成功した
ものである。即ち、洗浄中の温度（以下洗浄温度
という）を
(イ) Ｔ＞103−（13/12）Ｃ
Ｔ：温度（℃）
Ｃ：苛性ソーダ水溶液濃度（重量％）
(ロ) 苛性ソーダ水溶液の沸点未満の温度
(ハ) 80℃以上の温度
に維持することにより本発明の目的が充分に達せ
られることを見出したものである。 The present inventors have made repeated efforts to overcome the above-mentioned drawbacks, and have succeeded in solving this problem by cleaning with a caustic soda aqueous solution under specific conditions. That is, the temperature during cleaning (hereinafter referred to as cleaning temperature) is (a) T>103-(13/12)C T: Temperature (°C) C: Concentration of caustic soda aqueous solution (wt%) (b) Below the boiling point of the caustic soda aqueous solution Temperature (c) It has been found that the object of the present invention can be fully achieved by maintaining the temperature at 80°C or higher.
無水炭酸ソーダは、従来行なわれている軽灰を
１水塩化し、これを加熱分解して製造する方法、
あるいは特開昭55−7530号、特開昭56−109818
号、特開昭56−109819号等で開示される水溶液反
応による方法等が考えられる。前者の方法による
場合、通常STD（Steam−Tubed Dryer）と称せ
られる乾燥器で炭酸ソーダ１水塩を熱分解して無
水炭酸ソーダ結晶を得ているが、この方法による
場合は炭酸ソーダ１水塩を母液から分離するに際
し、母液中不純物濃度を調節したり、あるいは水
にて洗浄することで、製品中不純物濃度を調節す
ることが可能であるが、後者の場合は、炭酸ソー
ダ無水塩を析出させる条件から母液中のNaCl濃
度が限定されていたり、また、水にて洗浄した場
合は瞬時に分離機内にて水和反応により固結し、
無水のケーキを得ることができない。 Anhydrous soda carbonate is produced by the conventional method of converting light ash into monohydrate and thermally decomposing it.
Or JP-A-55-7530, JP-A-56-109818
Possible methods include methods using an aqueous solution reaction disclosed in Japanese Patent Application Laid-Open No. 109819/1983. In the former method, anhydrous sodium carbonate crystals are obtained by thermally decomposing sodium carbonate monohydrate in a dryer called an STD (Steam-Tubed Dryer); however, in this method, sodium carbonate monohydrate is When separating the product from the mother liquor, it is possible to adjust the impurity concentration in the product by adjusting the impurity concentration in the mother liquor or washing with water, but in the latter case, sodium carbonate anhydrous salt is precipitated. If the concentration of NaCl in the mother liquor is limited due to the conditions in which it is used, or if it is washed with water, it will instantly solidify in the separator due to a hydration reaction.
Can't get anhydrous cake.
従つて、上記現象の生じない方法として、本発
明者は鋭意検討を加えた結果、本発明をなしえた
もので、特定条件下で苛性ソーダ水溶液で洗浄す
ることを要旨とするものである。 Therefore, as a result of intensive studies, the present inventors have completed the present invention as a method that does not cause the above-mentioned phenomenon, and the gist thereof is to wash with a caustic soda aqueous solution under specific conditions.
無水炭酸ソーダ結晶を乾燥する場合、無水炭酸
ソーダ結晶を上述の法浄温度条件下に維持しなが
ら苛性ソーダ水溶液で洗浄することが必要であ
る。 When drying anhydrous sodium carbonate crystals, it is necessary to wash the anhydrous sodium carbonate crystals with an aqueous caustic soda solution while maintaining the crystals under the above-mentioned cleaning temperature conditions.
ここで洗浄温度とは、厳密には無水炭酸ソーダ
結晶の表面温度をいうが、無水炭酸ソーダ結晶が
上述の後者の方法で製造された製造直後のものの
場合には、この洗浄温度は、ほぼ近似的に洗浄液
である苛性ソーダ水溶液の温度と考えてよい。 Strictly speaking, the washing temperature here refers to the surface temperature of the anhydrous soda crystals, but if the anhydrous soda crystals have just been produced by the latter method mentioned above, the washing temperature is approximately the same. It can be thought of as the temperature of the caustic soda aqueous solution, which is the cleaning liquid.
洗浄温度が、上述の(イ)の条件を満たさない場合
は、無水炭酸ソーダ結晶の表面に炭酸ソーダ１水
塩が生成することがあるため、不適当である。洗
浄温度が上述の(ロ)の条件を満たない場合は、洗浄
液が沸騰するので不適当である。洗浄温度が上述
の(ハ)の条件を満たさない場合は、洗浄の速度が遅
く効率的な操作が困難であるので不適当である。 If the washing temperature does not satisfy the above-mentioned condition (a), it is inappropriate because sodium carbonate monohydrate may be formed on the surface of the anhydrous sodium carbonate crystals. If the cleaning temperature does not satisfy the above condition (b), the cleaning liquid will boil, which is inappropriate. If the cleaning temperature does not satisfy the above-mentioned condition (c), it is unsuitable because the cleaning speed is slow and efficient operation is difficult.
本発明は上述の洗浄条件の維持を必須条件とす
るが、洗浄後の無水炭酸ソーダ結晶の表面には洗
浄液である苛性ソーダ水溶液の薄い被膜が形成さ
れており、苛性ソーダが不純物として残る可能性
がある。かような苛性ソーダも不純物として許容
しえない時は、上記苛性ソーダ水溶液の被膜が付
着した無水炭酸ソーダ結晶を炭酸ガス又は炭酸ガ
スを含むガスで乾燥するとよい。 Although the present invention requires maintenance of the above-mentioned cleaning conditions, a thin film of aqueous caustic soda solution, which is the cleaning liquid, is formed on the surface of the anhydrous soda crystal after cleaning, and there is a possibility that caustic soda may remain as an impurity. . When such caustic soda cannot be tolerated as an impurity, it is preferable to dry the anhydrous soda crystals coated with the above caustic soda aqueous solution with carbon dioxide gas or a gas containing carbon dioxide gas.
この乾燥の場合にも、無水炭酸ソーダ結晶表面
に付着する苛性ソーダの濃度に関して上述の洗浄
温度条件下を維持することが必要である。 In this drying as well, it is necessary to maintain the above-mentioned washing temperature conditions regarding the concentration of caustic soda adhering to the anhydrous soda crystal surface.
即ち、付着母液が上述の洗浄温度条件下にある
場合は、炭酸ガス又は炭酸ガスを含むガスで乾燥
するにつれて、表面の苛性ソーダ水溶液は水分が
蒸発すると同時に、苛性ソーダが炭酸ガスと反応
して炭酸ソーダに変り、無水炭酸ソーダ結晶とし
て表面に析出固着する。 That is, when the adhering mother liquor is under the above-mentioned cleaning temperature conditions, as it is dried with carbon dioxide gas or a gas containing carbon dioxide gas, the water in the caustic soda aqueous solution on the surface evaporates, and at the same time, the caustic soda reacts with carbon dioxide gas to form sodium carbonate. , and precipitates and adheres to the surface as anhydrous sodium carbonate crystals.
乾燥及び反応の進行につれて、無水炭酸ソーダ
結晶の表面にある苛性ソーダ濃度は急激に減少す
るため、乾燥温度はそれに伴い上述の洗浄温度条
件、特に(イ)の条件を維持するように上昇せしめね
ばならない。しかしながら、乾燥の進行につれて
乾燥温度を変えることは実際的ではなく、実際に
工業的に実施する場合には炭酸ガス又は炭酸ガス
を含むガスの温度を103℃以上とするのがよい。 As the drying and reaction proceed, the concentration of caustic soda on the surface of the anhydrous sodium carbonate crystals rapidly decreases, so the drying temperature must be increased accordingly to maintain the above-mentioned washing temperature conditions, especially the condition (a). . However, it is not practical to change the drying temperature as the drying progresses, and in actual industrial implementation, it is preferable to set the temperature of carbon dioxide gas or a gas containing carbon dioxide gas to 103° C. or higher.
以上、説明した本発明方法によれば、洗浄液で
ある苛性ソーダ水溶液は循環使用が可能であるこ
とから、無水炭酸ソーダ結晶の歩留に悪影響は与
えないし、また、乾燥に使用する炭酸ガス又は炭
酸ガスを含むガスとして亜硫酸ガスを除去した工
業燃焼ガスが（必要に応じて若干加熱することに
より）使用可能であることから真に工業的に効果
の大なる方法であることが分る。 According to the method of the present invention described above, since the caustic soda aqueous solution that is the cleaning liquid can be reused, it does not have an adverse effect on the yield of anhydrous sodium carbonate crystals, and the carbon dioxide or carbon dioxide gas used for drying It can be seen that this is a truly industrially effective method since industrial combustion gas from which sulfur dioxide gas has been removed can be used as the gas containing sulfur dioxide (slightly heated if necessary).
また、使用する苛性ソーダ水溶液は、求める製
品純度に応じて多少の不純物が含まれていてもよ
いことは勿論である。 Further, it goes without saying that the caustic soda aqueous solution used may contain some impurities depending on the desired product purity.
以下、実施例により本発明を更に詳しく説明す
る。 Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例
塩安ソーダ法で得られる重曹、49％苛性ソーダ
水溶液及び食塩を反応容器にて、105℃、１気圧
で反応させ無水炭酸ソーダ結晶とNaCl15wt％、
Na2CO314.6％の母液からなるスラリーを得た。
この結晶を過により分離した無水炭酸ソーダ結
晶の表面には食塩が0.6％付着していた。Example: Baking soda obtained by the ammonium chloride method, 49% caustic soda aqueous solution, and common salt were reacted in a reaction vessel at 105°C and 1 atm to form anhydrous sodium carbonate crystals, NaCl 15wt%,
A slurry consisting of a mother liquor of 14.6% Na 2 CO 3 was obtained.
This crystal was separated by filtration, and 0.6% of common salt was found to be attached to the surface of the anhydrous soda crystal.
次にこの結晶を98℃に保持しつつ、90℃、30％
の苛性ソーダ水溶液で洗浄し、ついでこれを109
℃の炭酸ガスで乾燥した。 Next, while holding this crystal at 98℃, 90℃, 30%
Wash with a caustic soda aqueous solution of
Dry with carbon dioxide gas at ℃.
表面に付着した苛性ソーダの部分は完全に無水
炭酸ソーダに変化し（炭酸ソーダ１水塩は存在せ
ず）、これは強固にもとの無水炭酸ソーダと１体
化しており、この部分が剥離、粉化することはな
かつた。また、表面の不純物の食塩は実質的に存
在しなかつた。 The part of the caustic soda that adhered to the surface completely changes to anhydrous soda carbonate (there is no carbonate monohydrate), and this is firmly integrated with the original anhydrous carbonate soda, and this part peels off. It did not turn into powder. In addition, there was substantially no salt as an impurity on the surface.
比較例
実施例と同様にして得られた食塩を含む無水炭
酸ソーダ結晶を90℃、11％の苛性ソーダ水溶液に
て洗浄したところ、結晶表面の１部は炭酸ソーダ
１水塩に変り、たちまち、粒子同志が固結し、ブ
ロツク状となつた。Comparative Example When anhydrous sodium carbonate crystals containing salt obtained in the same manner as in the examples were washed with an 11% caustic soda aqueous solution at 90°C, part of the crystal surface turned into sodium carbonate monohydrate, and particles immediately formed. The comrades solidified into a block.
Claims (1)
温度を次の(イ)(ロ)(ハ)を同時に満足するように維持し
つつ、苛性ソーダ水溶液で洗浄することを特徴と
する無水炭酸ソーダ結晶の洗浄方法。 (イ) Ｔ＞103−（13/12）Ｃ Ｔ：温度（℃） Ｃ：苛性ソーダ水溶液濃度（重量％） (ロ) 苛性ソーダ水溶液の沸点未満の温度 (ハ) 80℃以上の温度 ２ 洗浄ののち、炭酸ガス又は炭酸ガスを含む雰
囲気で乾燥する特許請求の範囲第１項の無水炭酸
ソーダ結晶の洗浄方法。[Scope of Claims] 1. Anhydrous soda carbonate crystals are washed with a caustic soda aqueous solution while maintaining the washing temperature so as to simultaneously satisfy the following (a), (b), and (c). Method for cleaning anhydrous soda crystals. (a) T>103-(13/12)C T: Temperature (°C) C: Concentration of caustic soda aqueous solution (wt%) (b) Temperature below the boiling point of the caustic soda aqueous solution (c) Temperature over 80°C 2 After cleaning 2. The method of cleaning anhydrous sodium carbonate crystals according to claim 1, which comprises drying in carbon dioxide gas or an atmosphere containing carbon dioxide gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11923281A JPS5826027A (en) | 1981-07-31 | 1981-07-31 | Washing method for anhydrous sodium carbonate crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11923281A JPS5826027A (en) | 1981-07-31 | 1981-07-31 | Washing method for anhydrous sodium carbonate crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5826027A JPS5826027A (en) | 1983-02-16 |
| JPS6363485B2 true JPS6363485B2 (en) | 1988-12-07 |
Family
ID=14756226
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11923281A Granted JPS5826027A (en) | 1981-07-31 | 1981-07-31 | Washing method for anhydrous sodium carbonate crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5826027A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0740139B2 (en) * | 1987-05-20 | 1995-05-01 | 帝人株式会社 | Film for electrophotography |
-
1981
- 1981-07-31 JP JP11923281A patent/JPS5826027A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5826027A (en) | 1983-02-16 |
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