CN102329220A - Method for preparing calcium formate coproduced with calcium chloride and calcium hydroxide from chloroform leftovers - Google Patents
Method for preparing calcium formate coproduced with calcium chloride and calcium hydroxide from chloroform leftovers Download PDFInfo
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- CN102329220A CN102329220A CN201110142277A CN201110142277A CN102329220A CN 102329220 A CN102329220 A CN 102329220A CN 201110142277 A CN201110142277 A CN 201110142277A CN 201110142277 A CN201110142277 A CN 201110142277A CN 102329220 A CN102329220 A CN 102329220A
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- calcium
- chloroform
- calcium chloride
- formiate
- tankage
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Abstract
The invention provides a method for preparing calcium formate coproduced with calcium chloride and calcium hydroxide from chloroform leftovers. The method comprises the following steps of: diluting and dissolving chloroform leftovers with water, and leaching soluble substances out to obtain a chloroform leftover leach liquor; feeding the a chloroform leftover leach liquor into a reduced pressure distiller for distilling under reduced pressure, and separating calcium formate crystals out and filtering the chloroform leftovers in hot state when calcium formate reaches a supersaturating concentration while the concentration of calcium chloride is lower than a supersaturating concentration at the same temperature to obtain calcium formate crystals and a first filtrate; drying the formate crystals and smashing to obtain a calcium formate product; and feeding the first filtrate, distilling under reduced pressure, and separating calcium chloride and sodium chloride products. According to the method, pollution caused by chloroform leftovers is reduced effectively, products such as calcium formate, sodium hydroxide, calcium chloride and the like are developed, and a remarkable economic benefit is created.
Description
Technical field
The invention belongs to the technical field of organic chemistry three industrial wastes comprehensive utilization, relate in particular to the comprehensive utilization of chloroform tankage, particularly, relate to a kind of method of making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage.
Background technology
Adopt trichoro-aldehyde and lime to carry out alkaline hydrolysis in the industry and produce trichloromethane (chloroform), the chloroform of generation is steamed manufactures product, and remaining is exactly the chloroform tankage, is commonly called as lime cream.The staple of lime cream is calcium formiate (sub product), lime (excess raw material) and calcium chloride etc.According to calculating one ton of chloroform of every production, can produce 0.5 ton of calcium formiate.Calcium formiate is a kind of industrial chemicals of preciousness, and lime cream Chang Zuowei waste disposal, so not only waste resource, also contaminate environment.
The chloroform tankage through leaching after, after extracting the material of solubility, obtain chloroform tankage leaching liquid; Its staple is a calcium formiate; Calcium chloride and calcium hydroxide, wherein the content of calcium formiate is 130-170 gram/L, calcium chloride content is 40-60 gram/L; Calcium hydroxide content is 2 gram/L, also contains the sodium-chlor of minute quantity.Chloroform tankage leaching liquid is researched and developed products such as making calcium formiate, calcium chloride, calcium hydroxide will have very big economic worth.
Summary of the invention
The invention provides a kind of with the method for making calcium formiate coproduction sodium hydroxide and sodium-chlor with the chloroform tankage; This method has effectively been administered the pollution of chloroform tankage; Also develop products such as calcium formiate, sodium hydroxide and calcium chloride, created tangible economic benefit.
Technical scheme of the present invention is following: a kind of method of making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage; Comprise the steps; Chloroform tankage dilute with water is dissolved; Amount of water is controlled at and makes calcium formiate not be higher than 160g/L in the concentration of feed liquid, and postprecipitation to the solution that stirs is divided into supernatant liquid and lower sediment thing; Separate supernatant liquid and lower sediment thing, supernatant liquid is chloroform tankage leach liquor, and wherein the content of calcium formiate is 130-170 gram/L, and calcium chloride content is 40-60 gram/L, and calcium hydroxide content is 2 gram/L, also contains the sodium-chlor of minute quantity; Chloroform tankage leach liquor is sent in the underpressure distillation device; Stir, be heated to 20-100 ℃, and with the negative pressure of 400-420 mmhg under underpressure distillation; When calcium formiate reaches supersaturation concentration; And the concentration of calcium chloride is when being lower than the saturation concentration under this temperature, and the calcium formiate crystallization is separated out chloroform tankage leach liquor filtered while hot, obtains the calcium formiate crystal and first filtrating; The calcium formiate crystal is dry, obtains the calcium formiate product after the pulverizing; First filtrating is sent into the underpressure distillation device and is carried out underpressure distillation, when distillate reaches the calcium chloride saturated solution, sends into the water cooler crystallisation by cooling, and crystallization of calcium chloride is separated out and obtained calcium chloride crystal and residual solution, behind the calcium chloride crystal crushing packing, obtains the calcium chloride product; Contain sodium-chlor in the residual solution, through degree of depth distillation, cooling, crystallization obtains the sodium-chlor product.
The principle of technique scheme is: in 20-100 ℃ TR, the solubleness of calcium formiate in water is the 1/5-1/8 of calcium chloride, and along with the rising of temperature; The changes in solubility of calcium formiate is little; And the solubleness of calcium chloride obviously rises, therefore, and the control evaporation capacity of moisture content; The calcium formiate crystallization is separated out and, calcium chloride is still in solution.Then, utilize the difference different and content in first filtrating of calcium chloride and sodium-chlor solubleness size in the aqueous solution again, calcium chloride is separated with sodium-chlor.
Beneficial effect of the present invention is: the method for making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage according to the invention; Effectively administered the pollution of chloroform tankage; Also develop products such as sodium formiate, calcium formiate, formate, created tangible economic benefit.
Embodiment
Embodiment 1:
A kind of method of making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage; Comprise the steps; 500kg chloroform tankage dilute with water is dissolved; Amount of water is controlled at and makes calcium formiate not be higher than 160g/L in the concentration of feed liquid, and postprecipitation to the solution that stirs is divided into supernatant liquid and lower sediment thing; Separate supernatant liquid and lower sediment thing, supernatant liquid is chloroform tankage leach liquor, and wherein the content of calcium formiate is 150 gram/L, and calcium chloride content is 50 gram/L, and calcium hydroxide content is 2 gram/L, also contains the sodium-chlor of minute quantity; Chloroform tankage leach liquor is sent in the underpressure distillation device; Stir, be heated to 60 ℃, and with the negative pressure of 410 mmhg under underpressure distillation; When calcium formiate reaches supersaturation concentration; And the concentration of calcium chloride is when being lower than the saturation concentration under this temperature, and the calcium formiate crystallization is separated out chloroform tankage leach liquor filtered while hot, obtains the calcium formiate crystal and first filtrating; The calcium formiate crystal is dry, obtains the calcium formiate product after the pulverizing, and its calcium formiate that contains is 300kg; First filtrating is sent into the underpressure distillation device and is carried out underpressure distillation; When distillate reaches the calcium chloride saturated solution, send into the water cooler crystallisation by cooling, crystallization of calcium chloride is separated out and is obtained calcium chloride crystal and residual solution; The calcium chloride crystal obtains the calcium chloride product after pulverizing, packing, and its calcium chloride that contains is 90kg; Contain sodium-chlor in the residual solution, through degree of depth distillation, cooling, crystallization obtains the sodium-chlor product, and its sodium-chlor that contains is 2kg.
Embodiment 2:
A kind of method of making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage; Comprise the steps; 500kg chloroform tankage dilute with water is dissolved; Amount of water is controlled at and makes calcium formiate not be higher than 160g/L in the concentration of feed liquid, and postprecipitation to the solution that stirs is divided into supernatant liquid and lower sediment thing; Separate supernatant liquid and lower sediment thing, supernatant liquid is chloroform tankage leach liquor, and wherein the content of calcium formiate is 130 gram/L, and calcium chloride content is 40 gram/L, and calcium hydroxide content is 2 gram/L, also contains the sodium-chlor of minute quantity; Chloroform tankage leach liquor is sent in the underpressure distillation device; Stir, be heated to 20 ℃, and with the negative pressure of 400 mmhg under underpressure distillation; When calcium formiate reaches supersaturation concentration; And the concentration of calcium chloride is when being lower than the saturation concentration under this temperature, and the calcium formiate crystallization is separated out chloroform tankage leach liquor filtered while hot, obtains the calcium formiate crystal and first filtrating; The calcium formiate crystal is dry, obtains the calcium formiate product after the pulverizing, and its calcium formiate that contains is 250kg; First filtrating is sent into the underpressure distillation device and is carried out underpressure distillation, when distillate reaches the calcium chloride saturated solution, sends into the water cooler crystallisation by cooling; Crystallization of calcium chloride is separated out and is obtained calcium chloride crystal and residual solution; Behind the calcium chloride crystal crushing packing, obtain the calcium chloride product, its calcium chloride that contains is 70kg; Contain sodium-chlor in the residual solution, through degree of depth distillation, cooling, crystallization obtains the sodium-chlor product, and its sodium-chlor that contains is 2kg.
Embodiment 3
A kind of method of making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage; Comprise the steps; 500kg chloroform tankage dilute with water is dissolved; Amount of water is controlled at and makes calcium formiate not be higher than 160g/L in the concentration of feed liquid, and postprecipitation to the solution that stirs is divided into supernatant liquid and lower sediment thing; Separate supernatant liquid and lower sediment thing, supernatant liquid is chloroform tankage leach liquor, and wherein the content of calcium formiate is 170 gram/L, and calcium chloride content is 60 gram/L, and calcium hydroxide content is 2 gram/L, also contains the sodium-chlor of minute quantity; Chloroform tankage leach liquor is sent in the underpressure distillation device; Stir, be heated to 100 ℃, and with the negative pressure of 420 mmhg under underpressure distillation; When calcium formiate reaches supersaturation concentration; And the concentration of calcium chloride is when being lower than the saturation concentration under this temperature, and the calcium formiate crystallization is separated out chloroform tankage leach liquor filtered while hot, obtains the calcium formiate crystal and first filtrating; The calcium formiate crystal is dry, obtains the calcium formiate product after the pulverizing, and its calcium formiate that contains is 330kg; First filtrating is sent into the underpressure distillation device and is carried out underpressure distillation; When distillate reaches the calcium chloride saturated solution, send into the water cooler crystallisation by cooling, crystallization of calcium chloride is separated out and is obtained calcium chloride crystal and residual solution; Obtain the calcium chloride product behind the calcium chloride crystal crushing packing, its calcium chloride that contains is 110kg; Contain sodium-chlor in the residual solution, through degree of depth distillation, cooling, crystallization obtains the sodium-chlor product, and its sodium-chlor that contains is 2kg.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (1)
1. method of making calcium formiate co-product calcium chloride and calcium hydroxide with the chloroform tankage; It is characterized in that; Comprise the steps; With the dissolving of chloroform tankage dilute with water, amount of water is controlled at and makes calcium formiate not be higher than 160g/L in the concentration of feed liquid, and postprecipitation to the solution that stirs is divided into supernatant liquid and lower sediment thing; Separate supernatant liquid and lower sediment thing, supernatant liquid is chloroform tankage leach liquor, and wherein the content of calcium formiate is 130-170 gram/L, and calcium chloride content is 40-60 gram/L, and calcium hydroxide content is 2 gram/L, also contains the sodium-chlor of minute quantity; Chloroform tankage leach liquor is sent in the underpressure distillation device; Stir, be heated to 20-100 ℃, and with the negative pressure of 400-420 mmhg under underpressure distillation; When calcium formiate reaches supersaturation concentration; And the concentration of calcium chloride is when being lower than the saturation concentration under this temperature, and the calcium formiate crystallization is separated out chloroform tankage leach liquor filtered while hot, obtains the calcium formiate crystal and first filtrating; The calcium formiate crystal is dry, obtains the calcium formiate product after the pulverizing; First filtrating is sent into the underpressure distillation device and is carried out underpressure distillation, when distillate reaches the calcium chloride saturated solution, sends into the water cooler crystallisation by cooling, and crystallization of calcium chloride is separated out and obtained calcium chloride crystal and residual solution, obtains the calcium chloride product behind the calcium chloride crystal crushing packing; Contain sodium-chlor in the residual solution, through degree of depth distillation, cooling, crystallization obtains the sodium-chlor product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110142277A CN102329220A (en) | 2011-05-30 | 2011-05-30 | Method for preparing calcium formate coproduced with calcium chloride and calcium hydroxide from chloroform leftovers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110142277A CN102329220A (en) | 2011-05-30 | 2011-05-30 | Method for preparing calcium formate coproduced with calcium chloride and calcium hydroxide from chloroform leftovers |
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| CN102329220A true CN102329220A (en) | 2012-01-25 |
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| CN201110142277A Pending CN102329220A (en) | 2011-05-30 | 2011-05-30 | Method for preparing calcium formate coproduced with calcium chloride and calcium hydroxide from chloroform leftovers |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4327070A (en) * | 1980-08-08 | 1982-04-27 | Trw Inc. | Production of potassium formate from potassium sulfate |
| CN1153767A (en) * | 1995-12-09 | 1997-07-09 | 陈广生 | Formic acid and sodium sulfate producing method |
-
2011
- 2011-05-30 CN CN201110142277A patent/CN102329220A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4327070A (en) * | 1980-08-08 | 1982-04-27 | Trw Inc. | Production of potassium formate from potassium sulfate |
| CN1153767A (en) * | 1995-12-09 | 1997-07-09 | 陈广生 | Formic acid and sodium sulfate producing method |
Non-Patent Citations (3)
| Title |
|---|
| 付福余等: "回收氯仿碱解残夜生产甲酸钙", 《氯碱工业》 * |
| 吴树珍: "利用氯仿下脚料生产甲酸钠", 《化工环保》 * |
| 龙小兵等: "利用氯仿废渣水中甲酸钙制甲酸钠的研究", 《湖南化工》 * |
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Address after: 523000, room five, building 508, Jinhai building, Dongcheng District Tong Road, Dongguan, Guangdong Applicant after: Wang Jiaxing Address before: Wushi Village Primary School in Dongguan city of Dongcheng District province Guangdong road 523000 Lane 1 No. 6 main mountain Applicant before: Wang Jiaxing |
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Application publication date: 20120125 |