JPH0314777B2 - - Google Patents
Info
- Publication number
- JPH0314777B2 JPH0314777B2 JP58055306A JP5530683A JPH0314777B2 JP H0314777 B2 JPH0314777 B2 JP H0314777B2 JP 58055306 A JP58055306 A JP 58055306A JP 5530683 A JP5530683 A JP 5530683A JP H0314777 B2 JPH0314777 B2 JP H0314777B2
- Authority
- JP
- Japan
- Prior art keywords
- refrigerant
- ammonium chloride
- concentration
- ammonium
- precipitation
- 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 - Lifetime
Links
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 84
- 239000003507 refrigerant Substances 0.000 claims description 46
- 235000019270 ammonium chloride Nutrition 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 239000012267 brine Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 16
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 16
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 12
- 239000001099 ammonium carbonate Substances 0.000 claims description 12
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 235000002639 sodium chloride Nutrition 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical group CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 239000004338 Dichlorodifluoromethane Substances 0.000 claims description 6
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical group FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 claims description 6
- 235000019404 dichlorodifluoromethane Nutrition 0.000 claims description 6
- VOPWNXZWBYDODV-UHFFFAOYSA-N Chlorodifluoromethane Chemical compound FC(F)Cl VOPWNXZWBYDODV-UHFFFAOYSA-N 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000001294 propane Substances 0.000 claims description 4
- 238000009834 vaporization Methods 0.000 claims description 4
- 230000008016 vaporization Effects 0.000 claims description 4
- 239000001282 iso-butane Substances 0.000 claims description 3
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 claims description 3
- 229940029284 trichlorofluoromethane Drugs 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 239000000243 solution Substances 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-N sodium;hydron;carbonate Chemical compound [Na+].OC(O)=O UIIMBOGNXHQVGW-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- UMNKXPULIDJLSU-UHFFFAOYSA-N dichlorofluoromethane Chemical compound FC(Cl)Cl UMNKXPULIDJLSU-UHFFFAOYSA-N 0.000 description 1
- 229940099364 dichlorofluoromethane Drugs 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Description
【発明の詳細な説明】
本発明は塩化アンモニウムの析出方法、特に塩
化アンモニウム（以下塩安という）と重曹との結
晶を交互に得る所謂塩安ソーダ法において、被析
出液に冷媒を直接接触せしめて塩安を析出せしめ
る方法に係るものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for precipitating ammonium chloride, particularly in the so-called ammonium chloride soda method in which crystals of ammonium chloride (hereinafter referred to as ammonium chloride) and sodium bicarbonate are alternately obtained, in which a refrigerant is brought into direct contact with the precipitating liquid. The invention relates to a method for precipitating ammonium chloride.
塩安分離母液に炭酸ガスを導入して重曹を析出
せしめ、これを分離した重曹分離母液にアンモニ
アと食塩とを添加して塩安を析出せしめるように
した所謂塩安ソーダ法における塩安析出工程は、
例えば重曹分離母液にアンモニアを添加し、冷却
して塩安の一部を析出せしめ、析出塩安を分離
し、或は分離することなく、次いで食塩を添加し
て塩安の溶解度の低下を利用して更に塩安を析出
せしめる方法、或は前記重曹分離母液にアンモニ
アと食塩とを添加し、冷却して塩安を析出せしめ
る方法が採用されている。 Ammonium chloride precipitation step in the so-called ammonium chloride soda method, in which carbon dioxide gas is introduced into the ammonium chloride separated mother liquor to precipitate baking soda, and ammonia and common salt are added to the separated sodium chloride mother liquor to precipitate ammonium chloride. teeth,
For example, ammonia is added to the sodium bicarbonate separated mother liquor, cooled to precipitate part of the ammonium chloride, and the precipitated ammonium chloride is separated, or without separation, and then common salt is added to take advantage of the decrease in the solubility of ammonium chloride. A method is adopted in which ammonium chloride is further precipitated by adding ammonia and common salt to the sodium bicarbonate separated mother liquor and cooling the mixture to precipitate ammonium chloride.
何れの場合においても冷却手段は、飽和状態に
保持された塩安被析出液が過飽和状態を呈するこ
とを利用して、塩安被析出液の一部をクーラーに
より結晶が析出する寸前の過飽和迄冷却し、これ
を元の被析出液貯槽に戻し、ここで過飽和分の塩
安を析出させるようにしている。 In either case, the cooling means takes advantage of the fact that the ammonium chloride precipitation solution maintained in a saturated state exhibits a supersaturated state, and cools a portion of the ammonium chloride precipitation solution using a cooler until it reaches supersaturation, just before crystals are precipitated. It is cooled and returned to the original precipitation liquid storage tank, where the supersaturated amount of ammonium chloride is precipitated.
この工程に用いられるクーラーは、通常冷却部
に冷却ジヤケツトを備えた外部からの間接冷却型
であり、構造が複雑である他、操作的にも温度の
制御が微妙であり、一部クーラー内で結晶が析出
して度々詰まりを生ずる為、通常かかるクーラー
を数台用意して比較的短時間で切り換えを行な
い、詰まりを掃除しつつ使用しているのが実状で
あり、操作的にも設備的にも必ずしも満足し得る
ものでなかつた。 The coolers used in this process are usually of the indirect cooling type from the outside with a cooling jacket in the cooling section, and in addition to having a complex structure, temperature control is delicate in operation, and some Because crystals precipitate and often cause blockages, the reality is that several such coolers are prepared and switched over in a relatively short period of time, and used while cleaning the blockages, which is both operational and equipment-efficient. However, it was not always satisfactory.
これに対し、本願出願人はフロン等の液態冷媒
を塩安被析出液中に直接導入し、液態冷媒の気化
熱によつて液を冷却し、塩安を析出せしめる手段
を提案した。（特公昭54−42840号公報参照）この
方法は、従来法の如く複雑な構造と煩雑な操作を
必要とせず、装置に不都合な詰まりを生ずること
も少なく、円滑な操作を長期にわたり安定して実
施し得る利点がある。 In response to this, the applicant of the present invention has proposed a method in which a liquid refrigerant such as fluorocarbon is directly introduced into the ammonium chloride precipitation solution, the liquid is cooled by the heat of vaporization of the liquid refrigerant, and ammonium chloride is precipitated. (Refer to Japanese Patent Publication No. 54-42840.) This method does not require complicated structures and complicated operations unlike conventional methods, is less likely to cause inconvenient clogging of the equipment, and ensures smooth and stable operation over a long period of time. There are benefits that can be implemented.
しかしながら、冷却を終えて装置外に取り出さ
れたガス状の冷媒は、これをそのまま廃棄するこ
とは経済的な見地から許されず、これを再び液化
せしめて再使用するのが普通である。 However, from an economic standpoint, it is not permissible to dispose of the gaseous refrigerant taken out of the device after cooling, and it is common practice to liquefy it again and reuse it.
この様なガス状の冷媒の液化手段としては、先
づ圧縮機を通し、次いで冷却器に導いて行なうの
が普通である。この場合、冷媒は圧縮機及び冷却
器内を直接通過させる為、これら機内に例えば油
分等が存在するとこれが冷媒中に溶け込み、かか
る冷媒を循環使用すると塩安若しくは好ましから
ざる不純物の混入を来たす虞れがある。 Generally, such a gaseous refrigerant is liquefied by first passing it through a compressor and then introducing it into a cooler. In this case, since the refrigerant is passed directly through the compressor and cooler, if oil, etc., is present in these machines, it will dissolve into the refrigerant, and if such refrigerant is used in circulation, there is a risk of contamination with ammonium chloride or other undesirable impurities. There is.
この為用いられる圧縮機や冷却器はかかる不純
物の混入がない特殊なものが要求され、必然的に
かなり高価な設備を用いねばならない欠点があ
る。 For this reason, the compressor and cooler used are required to be special and free from such impurities, which inevitably requires the use of fairly expensive equipment.
本発明者は、かかる欠点を排除し、入手容易で
且安価な汎用の装置を用い、ガス状の冷媒を再使
用可能な液態冷媒に転換させる手段を見出すこと
を目的として種々研究、検討した結果、冷却され
たブラインとガス状冷媒を直接接触せしめること
により、前記目的を達成し得ることを見出した。 The present inventor has conducted various studies and examinations with the aim of eliminating such drawbacks and finding a means to convert gaseous refrigerant into reusable liquid refrigerant using easily available and inexpensive general-purpose equipment. have discovered that this object can be achieved by bringing the cooled brine into direct contact with the gaseous refrigerant.
かくして本発明は、食塩、炭酸ガス、アンモニ
アを原料として重曹と塩化アンモニウムとを交互
に析出せしめる方法において、塩化アンモニウム
の析出を、被析出液中に直接液態冷媒を導入して
その気化熱により冷却することにより行ない、冷
却後の気化した冷媒を冷却したブラインと直接接
触せしめることにより再び液化し、これを塩化ア
ンモニウムの析出に循環使用する方法であつて、
該ブラインは水酸化アンモニウムおよび炭酸アン
モニウムの水溶液であり、その濃度を、冷媒の固
体水和物の生成濃度を超える濃度かつ炭酸アンモ
ニウムの溶解度未満の濃度に制御することを特徴
とする塩化アンモニウムの析出方法を提供するに
ある。 Thus, the present invention is a method in which baking soda and ammonium chloride are alternately precipitated using common salt, carbon dioxide gas, and ammonia as raw materials, in which the precipitation of ammonium chloride is cooled by directly introducing a liquid refrigerant into the precipitating liquid and using its heat of vaporization. A method in which the vaporized refrigerant after cooling is brought into direct contact with the cooled brine to liquefy it again, and this is recycled for use in the precipitation of ammonium chloride,
Precipitation of ammonium chloride, characterized in that the brine is an aqueous solution of ammonium hydroxide and ammonium carbonate, and its concentration is controlled to a concentration that exceeds the formation concentration of solid hydrate of the refrigerant and is less than the solubility of ammonium carbonate. We are here to provide you with a method.
本発明を採用する場合には、特別高価な冷却器
を必要とせず、汎用の冷却器を適宜用いることが
出来、しかもブラインの種類を選ぶことにより、
従来必要としていたガス状冷媒の圧縮機は必ずし
も必要としない利点がある。 When adopting the present invention, there is no need for a particularly expensive cooler, and a general-purpose cooler can be used as appropriate, and by selecting the type of brine,
It has the advantage that a compressor for gaseous refrigerant, which was conventionally required, is not necessarily required.
本発明に用いられる冷媒としては、これを直接
塩安の被析出溶液と接触せしめる関係上、塩安と
直接反応しないことは勿論、その他溶液中に含ま
れる他の成分とも実質的に反応しないことが望ま
しい。 Since the refrigerant used in the present invention is brought into direct contact with the ammonium chloride solution, it must not only not react directly with the ammonium chloride but also substantially not react with other components contained in the solution. is desirable.
この為、用いられる冷媒としては、例えばジク
ロロジフルオロメタン、トリクロロフルオロメタ
ン、クロルジフルオロメタン、プロパン、ｎ−ブ
タン、ｉ−ブタン等の液化され得る冷媒が挙げら
れるが、使用状態においてかなりの高圧が要求さ
れるものや、引火等の火災や爆発の危険性のある
ものは好ましくない。 For this reason, the refrigerants used include, for example, refrigerants that can be liquefied, such as dichlorodifluoromethane, trichlorofluoromethane, chlorodifluoromethane, propane, n-butane, and i-butane, but considerably high pressure is required under the conditions of use. It is undesirable to use items that may cause a fire or explosion due to ignition.
この為、これら冷媒のうち、ジクロロジフルオ
ロメタン、クロルジフルオロメタンは上記の如き
危険性がなく、又、特別な高圧を要することな
く、所期の目的を達成し得るので本発明に用いる
冷媒として特に好ましい。 Therefore, among these refrigerants, dichlorodifluoromethane and chlorodifluoromethane are particularly suitable as refrigerants for use in the present invention because they do not pose the above-mentioned dangers and can achieve the desired purpose without requiring special high pressure. preferable.
冷媒と接触せしめて塩安の被析出液を冷却する
温度は、塩安の析出量及び得ようとする塩安粒子
の大きさ等により任意に選択し得るが、例えば冷
媒としてジクロロジフルオロメタンを用い、析出
装置内圧2.4Kg／cm2Ｇ程度において５℃程度に冷
却することにより、粒径500〜2000μの塩安を析
出せしめることが出来る。他の冷媒を用いても０
〜15℃に冷却することにより、他の溶存成分、例
えば食塩、重曹等が共析せず、粒度等の特性にお
いて好ましい塩安を析出させることができる。冷
媒を塩安と被析出液と接触せしめるには、常温で
ガス状の冷媒を液化せしめ、これを例えば塩安を
析出せしめる槽、或は塩安の被析出液を導入した
冷却槽の下底付近より適当なノズルを用いて被析
出液中に微細な液滴として導入することにより、
これが被析出液中を上昇する間にガス化し、この
際液中から気化熱を奪い、冷却の目的が達成され
る。 The temperature at which the ammonium chloride precipitation solution is cooled by contacting with a refrigerant can be arbitrarily selected depending on the amount of ammonium chloride precipitated and the size of the ammonium chloride particles to be obtained, but for example, dichlorodifluoromethane may be used as the refrigerant. By cooling to about 5° C. at an internal pressure of about 2.4 kg/cm 2 G in the precipitation device, ammonium chloride having a particle size of 500 to 2000 μ can be precipitated. 0 even if other refrigerants are used
By cooling to ~15°C, other dissolved components such as common salt, sodium bicarbonate, etc. do not eutectoid, and ammonium chloride having preferable characteristics such as particle size can be precipitated. In order to bring the refrigerant into contact with ammonium chloride and the liquid to be precipitated, the refrigerant, which is gaseous at room temperature, is liquefied and used in a tank for precipitating ammonium chloride, or at the bottom of a cooling tank into which the liquid to be precipitated with ammonium chloride is introduced. By introducing fine droplets into the liquid to be precipitated using an appropriate nozzle from nearby,
While rising in the liquid to be precipitated, it gasifies, and at this time removes the heat of vaporization from the liquid, achieving the purpose of cooling.
かくしてガス化された少量のアンモニアガス、
炭酸ガス及び水蒸気を含有している冷媒は、析出
槽から取出され、本発明方法に従つて再び液化さ
れる。即ち、ガス化された冷媒は、冷却されたブ
ラインと直接接触せしめることにより液化を行な
う。ブラインの冷却手段に特に制限はなく、適宜
公知の手段を採用し得る。 A small amount of ammonia gas is thus gasified,
The refrigerant containing carbon dioxide gas and water vapor is removed from the precipitation tank and reliquefied according to the method of the invention. That is, the gasified refrigerant is liquefied by being brought into direct contact with the cooled brine. There is no particular restriction on the means for cooling the brine, and any known means may be employed as appropriate.
本発明のブラインは、水酸化アンモニウムおよ
び炭酸アンモニウムの水溶液である。そして、こ
の水溶液の濃度は冷却液化しようとする冷媒の種
類や必要とする温度等により、厳密には決定され
るが、冷媒の固体水和物の生成濃度を超える濃度
かつ炭酸アンモニウムの溶解度未満の濃度に制御
する必要がある。冷媒の固体水和物は、一般にブ
ライン濃度が次のＡで示される濃度を超える場合
には生成しない。 The brine of the present invention is an aqueous solution of ammonium hydroxide and ammonium carbonate. The concentration of this aqueous solution is strictly determined by the type of refrigerant to be liquefied, the required temperature, etc., but the concentration must be higher than the concentration of solid hydrate produced by the refrigerant and lower than the solubility of ammonium carbonate. It is necessary to control the concentration. Solid hydrates of refrigerants generally do not form when the brine concentration exceeds the concentration indicated by A below.
Ａ＝Ｘ−ｔ／0.57
Ａ：水酸化アンモニウム及び炭酸アンモニウム濃
度の合計値〔wt％〕
ｔ：冷却されたブラインの温度〔℃〕
ｘ：冷媒の種類によつて定まる定数
ジクロロジフルオロメタン＝12.6
トリフロロフルオロメタン＝6.8
クロロジフルオロメタン＝17.8
プロパン＝5.5
イソブタン＝1.8
ブラインの濃度がＡ以下の場合は、冷媒と水と
で固体の水和化合物を生じ、装置及び配管等を閉
塞させる原因となり、逆に濃度が高くなり過ぎ
て、炭酸アンモニウムの溶解度以上になると炭酸
アンモニウムの結晶が析出し、装置及び配管等を
閉塞させる虞れがあるので何れも不適当である。 A=X-t/0.57 A: Total value of ammonium hydroxide and ammonium carbonate concentration [wt%] t: Temperature of cooled brine [°C] x: Constant determined by the type of refrigerant dichlorodifluoromethane = 12.6 Tri Fluorofluoromethane = 6.8 Chlorodifluoromethane = 17.8 Propane = 5.5 Isobutane = 1.8 If the brine concentration is below A, the refrigerant and water will form a solid hydrated compound, which may cause blockage of equipment and piping, etc. If the concentration becomes too high and exceeds the solubility of ammonium carbonate, ammonium carbonate crystals may precipitate and clog the equipment, piping, etc., so either is inappropriate.
ブラインとガス状冷媒とを直接接触せしめる手
段に特に限定はなく、例えば充填塔、スプレー塔
等の装置や手段を適宜採用し得る。 There is no particular limitation on the means for bringing the brine and the gaseous refrigerant into direct contact, and for example, devices and means such as a packed tower and a spray tower may be appropriately employed.
なお、アンモニア水やアンモニアと炭酸ガスの
混合液をブラインとして用いる場合には、冷媒は
液態になつた際、容易に層状に分離されるので、
液態冷媒だけを容易に分取出来、再使用すること
が出来る。 Note that when using aqueous ammonia or a mixture of ammonia and carbon dioxide as brine, the refrigerant is easily separated into layers when it becomes liquid.
Only the liquid refrigerant can be easily separated and reused.
本発明においてガス状冷媒をブラインと直接接
触せしめて液化せしめる場合には、特に従来の様
に予めガス状冷媒を圧縮機により圧縮せしめる必
要はないが、所望により予め圧縮せしめておくこ
とも出来る。 In the present invention, when the gaseous refrigerant is brought into direct contact with brine and liquefied, it is not necessary to compress the gaseous refrigerant in advance with a compressor as in the conventional method, but it can be compressed in advance if desired.
次に本発明を実施例により説明する。 Next, the present invention will be explained by examples.
塩安ソーダ法を実施して得た析出重曹を分離し
た母液にアンモニアと食塩を添加して得た塩化ア
ンモニウム18wt％、食塩8wt％、炭酸アンモニウ
ム13wt％、水酸化アンモニウム1.5wt％を含む温
度30℃の水溶液0.5m3を析出槽に導入し、撹拌下
に析出槽下部より冷媒として液化したジクロロフ
ルオロメタンを50Kg／ｈの割合で導入し、槽内で
気化せしめて冷却を行なつた。ガス化した冷媒は
汎用の冷凍設備をもちいて０℃へ冷却された水酸
化アンモニウム13wt％、炭酸アンモニウム17wt
％を含む水溶液と充填塔で直接接触せしめること
により、再び液化せしめた。液化時の圧力は2.5
Kg／cm2Ｇであつた。液化した冷媒はブラインと容
易に層状に分離されるので液化した冷媒のみを取
り出し塩安析出槽へ再び循環使用した。 Temperature 30 containing 18 wt% ammonium chloride, 8 wt% common salt, 13 wt% ammonium carbonate, and 1.5 wt% ammonium hydroxide obtained by adding ammonia and common salt to the mother liquor from which the precipitated sodium bicarbonate obtained by carrying out the ammonium chloride method was separated. 0.5 m 3 of an aqueous solution at temperature was introduced into the precipitation tank, and while stirring, liquefied dichlorofluoromethane was introduced as a refrigerant from the bottom of the precipitation tank at a rate of 50 kg/h, and was vaporized in the tank for cooling. The gasified refrigerant contains 13wt% ammonium hydroxide and 17wt% ammonium carbonate, which are cooled to 0℃ using general-purpose refrigeration equipment.
% of the aqueous solution in a packed column, it was liquefied again. The pressure during liquefaction is 2.5
It was Kg/cm 2 G. Since the liquefied refrigerant was easily separated into layers from the brine, only the liquefied refrigerant was taken out and recycled to the ammonium chloride precipitation tank.
Claims (1)
曹と塩化アンモニウムとを交互に析出せしめる方
法において、塩化アンモニウムの析出を、被析出
液中に直接液態冷媒を導入してその気化熱により
冷却することにより行ない、冷却後の気化した冷
媒を冷却したブラインと直接接触せしめることに
より再び液化し、これを塩化アンモニウムの析出
に循環使用する方法であつて、該ブラインは水酸
化アンモニウムおよび炭酸アンモニウムの水溶液
であり、その濃度を冷媒の固体水和物の生成濃度
を超える濃度かつ炭酸アンモニウムの溶解度未満
の濃度に制御することを特徴とする塩化アンモニ
ウムの析出方法。 ２ 冷媒が、ジクロロジフルオロメタン、トリク
ロロフルオロメタン、クロロジフルオロメタン、
プロパン、イソブタンから選ばれるものであり、
水酸化アンモニウムおよび炭酸アンモニウムを含
む水溶液の濃度が、次式のＡで示される濃度を超
える特許請求の範囲第１項記載の塩化アンモニウ
ムの析出方法。 Ａ＝Ｘ−ｔ／0.57 Ａ：水酸化アンモニウムおよび炭酸アンモニウム
濃度の合計値［wt％］ ｔ：冷却されたブラインの温度［℃］ Ｘ：冷媒の種類によつて定まる定数 ジクロロジフルオロメタン＝12.6 トリクロロフルオロメタン＝6.8 クロロジフルオロメタン＝17.8 プロパン＝5.5 イソブタン＝1.8[Claims] 1. In a method of alternately precipitating baking soda and ammonium chloride using common salt, carbon dioxide gas, and ammonia as raw materials, the precipitation of ammonium chloride is carried out by introducing a liquid refrigerant directly into the liquid to be precipitated to reduce its heat of vaporization. After cooling, the vaporized refrigerant is brought into direct contact with cooled brine to liquefy it again, and this is recycled for use in the precipitation of ammonium chloride. A method for precipitating ammonium chloride, which is an aqueous solution of ammonium, and the concentration thereof is controlled to a concentration that exceeds the concentration of solid hydrate produced in a refrigerant and is lower than the solubility of ammonium carbonate. 2 The refrigerant is dichlorodifluoromethane, trichlorofluoromethane, chlorodifluoromethane,
It is selected from propane and isobutane,
The method for precipitating ammonium chloride according to claim 1, wherein the concentration of the aqueous solution containing ammonium hydroxide and ammonium carbonate exceeds the concentration represented by A in the following formula. A=X-t/0.57 A: Total value of ammonium hydroxide and ammonium carbonate concentration [wt%] t: Temperature of cooled brine [°C] X: Constant determined by the type of refrigerant Dichlorodifluoromethane = 12.6 Trichloro Fluoromethane = 6.8 Chlorodifluoromethane = 17.8 Propane = 5.5 Isobutane = 1.8
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5530683A JPS59184728A (en) | 1983-04-01 | 1983-04-01 | Precipitating method of ammonium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5530683A JPS59184728A (en) | 1983-04-01 | 1983-04-01 | Precipitating method of ammonium chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59184728A JPS59184728A (en) | 1984-10-20 |
| JPH0314777B2 true JPH0314777B2 (en) | 1991-02-27 |
Family
ID=12994880
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5530683A Granted JPS59184728A (en) | 1983-04-01 | 1983-04-01 | Precipitating method of ammonium chloride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59184728A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006090524A1 (en) | 2005-02-22 | 2006-08-31 | Shin-Etsu Chemical Co., Ltd. | Method for measuring non-circularity at core portion of optical fiber parent material |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942195A (en) * | 2012-11-23 | 2013-02-27 | 湖北双环科技股份有限公司 | Method for improving production capacity of crystallizer for co-production of ammonium chloride and soda ash |
| CN107585778A (en) * | 2017-10-15 | 2018-01-16 | 赵祥海 | Salting-out crystallizer outer loop cool-down method in procedure of producing soda under joint alkaline process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5423908A (en) * | 1977-07-22 | 1979-02-22 | Canon Inc | Vibration-proof for brush in rotary equipment |
| JPS5442840A (en) * | 1977-09-10 | 1979-04-05 | Baanaa Intaanashiyonaru Kk | Rotary dry moisture removing machine |
| JPS54157772A (en) * | 1978-06-01 | 1979-12-12 | Matsuko Shimokawa | Fresh water obtaining and concentrating method by freezing |
-
1983
- 1983-04-01 JP JP5530683A patent/JPS59184728A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5423908A (en) * | 1977-07-22 | 1979-02-22 | Canon Inc | Vibration-proof for brush in rotary equipment |
| JPS5442840A (en) * | 1977-09-10 | 1979-04-05 | Baanaa Intaanashiyonaru Kk | Rotary dry moisture removing machine |
| JPS54157772A (en) * | 1978-06-01 | 1979-12-12 | Matsuko Shimokawa | Fresh water obtaining and concentrating method by freezing |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006090524A1 (en) | 2005-02-22 | 2006-08-31 | Shin-Etsu Chemical Co., Ltd. | Method for measuring non-circularity at core portion of optical fiber parent material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59184728A (en) | 1984-10-20 |
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