CN105836764B - Recycling method of waste salt from salt-containing waste water in organic synthetic industry - Google Patents
Recycling method of waste salt from salt-containing waste water in organic synthetic industry Download PDFInfo
- Publication number
- CN105836764B CN105836764B CN201610174088.8A CN201610174088A CN105836764B CN 105836764 B CN105836764 B CN 105836764B CN 201610174088 A CN201610174088 A CN 201610174088A CN 105836764 B CN105836764 B CN 105836764B
- Authority
- CN
- China
- Prior art keywords
- salt
- dihydrogen phosphate
- solid
- sodium chloride
- saturated solution
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a recycling method of waste salt from salt-containing waste water in organic synthetic industry. The recycling method includes the steps of: evaporating the salt-containing waste water in the organic synthetic industry to obtain salt residue containing sodium chloride and sodium dihydrogen phosphate; eluting the salt residue and performing solid-liquid separation, preparing a saturated water solution of the salt residue at 80-90 DEG C from the separated solid, wherein residual undissolved salt residue is recycled and is repeatedly dissolved for more than 5 times to prepare sodium chloride; and cooling the saturated solution to 2-5 DEG C to crystallize the saturated solution to separate sodium dihydrogen phosphate. The industrial waste salt as the raw material is turned from waste into resources, so that the method is beneficial to environment protection and comprehensive utilization. The recycled sodium chloride and sodium dihydrogen phosphate are high in quality and has good crystal granularity. The method reaches more than 80% in recycling rate and more than 98% in product purity.
Description
Technical field
The invention belongs to energy-conserving and emission-cutting technology field, and in particular to the recovery side of abraum salt in organic synthesiss industry brine waste
Method.
Background technology
Sodium dihydrogen phosphate is a kind of important chemical products, has extensively use at aspects such as medicine, food, chemical industry, agriculturals
On the way.Industry Waste Sodium Chloride is that a kind of yield is big and intractable pollutant, and general processing method is dilution discharge, but can be caused
Serious land pollution.Document 1 carries out separating-purifying to halide salt using cool technology-floatation process, but what the method was obtained
Product quality is not high, and the response rate of halide salt is not ideal enough, and only 40%~50%, and in the multiple links of technological process such as ore deposit amount
Control, the misoperation decomposed in control, the addition of floating agent and washing etc. of the water yield all can cause product recovery rate not
Good impact (Zhang Yikui, the experimental study of potassium chloride and Sodium Chloride separating technology, sea lake salt and chemical industry in carnallite,
1994).Zheng Xueming et al. produces sodium dihydrogen phosphate using phosphoric acid and the reaction of Industry Waste Sodium Chloride, although can solve the problem that industrial chlorine
Change the pollution problem of sodium, and produce sodium dihydrogen phosphate, but technique needs to add extra concentrated acid to realize, equipment is set
Apply that requirement is higher, technological process is complex, and dealing with improperly can cause larger pollution (Zheng Xueming, industrial waste salt life to environment
The technical study of product sodium dihydrogen phosphate, the 26th Annual Conference Green Chemistry collection of thesis of Chemistry In China, 2008).Therefore, one is found
The saliferous waste residue in efficient recovery process organic industry synthetic wastewater is planted to environmental conservation and comprehensive utilization of waste materials with very heavy
The practical significance wanted.
The content of the invention
For the deficiencies in the prior art, the invention provides a kind of organic synthesiss industry brine waste in abraum salt recovery side
Method, can efficiently separate Sodium Chloride and sodium dihydrogen phosphate.
Technical scheme is as follows：
The recovery method of abraum salt, comprises the following steps that in a kind of organic synthesiss industry brine waste：
Step 1, the salt containing Sodium Chloride and sodium dihydrogen phosphate that organic synthesiss industry brine waste evaporation process is obtained
Slag solid-liquid separation after the process of organic solvent eluting, the solid being dried to obtain；
Step 2, dried salt slag in step 1 is soluble in water at 80 DEG C~90 DEG C, obtain Sodium Chloride and di(2-ethylhexyl)phosphate
The mixing saturated solution of hydrogen sodium, saturated solution is separated by filtration, and undissolved solid individually reclaims after being dried and repeats to dissolve, and repeats
Dissolving at least 5 times, repeats undissolved solid in the saturated solution after dissolving and is Sodium Chloride；
Step 3, will be separated by filtration the saturated solution that obtains and is cooled to 2 DEG C~5 DEG C in step 2, stand more than 2h, treat saturation
After salinity in solution is separated out completely, solid separated, be dried, obtain sodium dihydrogen phosphate, obtained after remaining liquid evaporation
Salt slag continues repeat step 2 and step 3.
Preferably, in step 1, described organic solvent is ethanol or chloroform.
Compared with prior art, the present invention turns waste into wealth with industrial waste salt slag as raw material, is conducive to environmentally friendly and comprehensive profit
With, process costs are low, reclaim that the product quality that obtains is high, and product crystalline substance position can reach more than 90%, reclaim obtain Sodium Chloride,
Sodium dihydrogen phosphate grain size is preferable, and the response rate can reach more than 80%, and product purity is up to more than 98%.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
With reference to embodiment and accompanying drawing, the invention will be further described.
With reference to Fig. 1, the recovery method of abraum salt, comprises the following steps that in a kind of organic synthesiss industry brine waste：
Step 1, the salt containing Sodium Chloride and sodium dihydrogen phosphate that organic synthesiss industry brine waste evaporation process is obtained
Slag solid-liquid separation after the process of organic solvent eluting, and the isolated solid of drying；
Step 2, dried salt slag in step 1 is soluble in water at 80 DEG C~90 DEG C, obtain Sodium Chloride and di(2-ethylhexyl)phosphate
The mixing saturated solution of hydrogen sodium, saturated solution is separated by filtration, and undissolved solid individually reclaims redissolution solution of laying equal stress on, weight after being dried
Redissolution solution at least 5 times, repeats undissolved solid in the saturated solution after dissolving and is Sodium Chloride；
Step 3, will be separated by filtration the saturated solution that obtains and is cooled to 2 DEG C~5 DEG C in step 2, stand more than 2h, treat saturation
After salinity in solution is separated out completely, solid separated, be dried, obtain sodium dihydrogen phosphate, obtained after remaining liquid evaporation
Salt slag continues repeat step 2 and step 3.
Preferably, in step 1, described organic solvent is ethanol or chloroform.
Embodiment 1
Step 1, the waste salt dregs chloroform of 500g that organic synthesiss industry brine waste evaporation process is obtained will remain organic
Thing carries out eluting process, subsequently carries out solid-liquid separation, and the solid after separation is dried in an oven at 90 DEG C.
Step 2, the salt slag after step 1 dried is dissolved in the water under conditions of 90 DEG C and prepares saturated salt solution,
Redissolution solution of laying equal stress on individually is reclaimed after solid without dissolving is separated by filtration, after at least 5 times repetitions are dissolved, is not had in solution
The solid of dissolving is Sodium Chloride.
Step 3, by the saturated salt solution being separated by filtration in step 22 DEG C are cooled to, and stand 2h, treat salt in saturated salt solution
Divide after separating out completely, solid is separated, is dried, obtain sodium dihydrogen phosphate, the salt slag obtained after unnecessary liquid evaporation continues heavy
Multiple step 2 and step 3.
After 2~step 3 of repeat step five times, the response rate is 87.4%, the purity point of Sodium Chloride and sodium dihydrogen phosphate
Wei 99% and 98%.
Embodiment 2
Step 1, the waste salt dregs of the 500g that organic synthesiss waste water evaporation process is obtained are washed residual organic matter with ethanol
It is de- to process, solid-liquid separation is subsequently carried out, the solid after separation is dried in an oven at 90 DEG C.
Step 2, the salt slag after dried is dissolved in the water under conditions of 80 DEG C and prepares saturated salt solution, will not had
The solid of dissolving repeatedly dissolves after individually reclaiming after being separated by filtration, after at least 5 times are processed, without the solid of dissolving in solution
As Sodium Chloride.
Step 3, by the saturated salt solution obtained in step 25 DEG C are cooled to, and stand 2h, treat that salinity is complete in saturated salt solution
After full precipitation, solid is separated, is dried, just obtain sodium dihydrogen phosphate, the salt slag obtained after unnecessary liquid evaporation continues to repeat
Step 2.
After 2~step 3 of repeat step five times, the response rate is 80.2%.The purity of Sodium Chloride and sodium dihydrogen phosphate is equal
For 98%.
Claims (1)
1. in a kind of organic synthesiss industry brine waste abraum salt recovery method, it is characterised in that comprise the following steps that：
Step 1, the salt slag containing Sodium Chloride and sodium dihydrogen phosphate that organic synthesiss industry brine waste evaporation process is obtained is used
Solid-liquid separation after the process of organic solvent eluting, the solid being dried to obtain, described organic solvent is ethanol or chloroform；
Step 2, dried salt slag in step 1 is soluble in water at 80 DEG C~90 DEG C, obtain Sodium Chloride and sodium dihydrogen phosphate
Mixing saturated solution, saturated solution is separated by filtration, undissolved solid individually reclaims after being dried and repeats to dissolve, and repeats to dissolve
At least 5 times, repeat undissolved solid in the saturated solution after dissolving and be Sodium Chloride；
Step 3, will be separated by filtration the saturated solution that obtains and is cooled to 2 DEG C~5 DEG C in step 2, stand more than 2h, treat saturated solution
In salinity separate out completely after, by solid separate, be dried, obtain sodium dihydrogen phosphate, the salt slag obtained after remaining liquid evaporation
Continue repeat step 2 and step 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610174088.8A CN105836764B (en) | 2016-03-24 | 2016-03-24 | Recycling method of waste salt from salt-containing waste water in organic synthetic industry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610174088.8A CN105836764B (en) | 2016-03-24 | 2016-03-24 | Recycling method of waste salt from salt-containing waste water in organic synthetic industry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105836764A CN105836764A (en) | 2016-08-10 |
| CN105836764B true CN105836764B (en) | 2017-05-17 |
Family
ID=56583296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610174088.8A Active CN105836764B (en) | 2016-03-24 | 2016-03-24 | Recycling method of waste salt from salt-containing waste water in organic synthetic industry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105836764B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455741B (en) * | 2018-11-29 | 2020-04-28 | 华南理工大学 | Method for recycling and fully utilizing sodium chloride waste salt slag by using low-temperature roasting and interface regulation and control |
| CN109607503A (en) * | 2018-12-27 | 2019-04-12 | 南京理工大学 | Phosphatic abraum salt recycling processing method |
| CN109911918B (en) * | 2019-05-07 | 2021-07-30 | 江苏迈克化工机械有限公司 | Resource utilization method of industrial mixed salt containing organic solvent |
| CN114933288B (en) * | 2022-04-28 | 2023-05-19 | 四川轻化工大学 | High-purity potassium dihydrogen phosphate and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2260975B (en) * | 1991-10-28 | 1995-07-12 | Chang Shih Chang | The process to recover salt from brine waste water |
| CN100413786C (en) * | 2005-11-22 | 2008-08-27 | 宜宾天原集团股份有限公司 | Process for treating hydrazine hydrate waste salt water by ketone linking nitrogen method |
| CN102849755B (en) * | 2012-10-17 | 2014-04-02 | 安徽理工大学 | Purification method for industrial byproduct salt and purification device therefor |
| CN104291523A (en) * | 2014-09-18 | 2015-01-21 | 波鹰(厦门)科技有限公司 | Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater |
| CN105036155B (en) * | 2015-07-24 | 2016-08-24 | 杭州天创环境科技股份有限公司 | The refining technique of by-product salt on a kind of glyphosate production route |
-
2016
- 2016-03-24 CN CN201610174088.8A patent/CN105836764B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105836764A (en) | 2016-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105836764B (en) | Recycling method of waste salt from salt-containing waste water in organic synthetic industry | |
| CN102557085B (en) | Method for extracting sodium salt in cesium salt and rubidium salt production process | |
| CN102531025B (en) | Method for treating rare earth ammonium chloride wastewater | |
| CN101905942B (en) | Method for treating condensed mother solution of azodicarbonamide foaming agent | |
| CN106587105A (en) | Method for recovering copper chloride acid etching liquid in printed circuit board | |
| CN109607503A (en) | Phosphatic abraum salt recycling processing method | |
| CN104649300A (en) | Method for recovering and refining sodium bromide from dipropyl cyanoacetate mixture | |
| CN106185810A (en) | A kind of joint disposal technique of acidic copper chloride waste etching solution | |
| CN108288737B (en) | Method for recovering lithium hexafluorophosphate from waste lithium battery cathode material | |
| CN104591486B (en) | A kind of processing method of Low acid dye wastewater | |
| CN107117760A (en) | A kind of method for removing organic matter in automobile industry water soluble dyestuffs coating waste-water | |
| CN104844469A (en) | Clean production technology of methyl anthranilate | |
| EP3611736A1 (en) | Method for treating liquid waste from a nuclear power plant with boron control | |
| KR20180064753A (en) | Methods for waste water treatment of Nitrogen trifluoride(NF3) process | |
| CN109455741B (en) | Method for recycling and fully utilizing sodium chloride waste salt slag by using low-temperature roasting and interface regulation and control | |
| CN103130296B (en) | Acetate-containing industrial organic wastewater treatment process | |
| CN113955772B (en) | Separation and purification method of fly ash water-washed soluble chloride salt | |
| CN102451916A (en) | Method for transforming aqueous solution containing copper chloride into copper powder and polyaluminum chloride (PAC) | |
| CN108484423A (en) | A method of isolating and purifying l-Alanine from l-Alanine zymotic fluid | |
| CN105417584A (en) | Method for recycling manganese from electrolyzed manganese ore residues | |
| CN103435070B (en) | A kind of from containing the method reclaiming product the waste residue of Sodium Fluoride | |
| CN106044868A (en) | Technological method and device for preparing ferrous sulfate crystals by aid of copper sulfate waste liquor | |
| CN104609442A (en) | Method for recycling waste residues produced by synthesis of TAIC (triallyl isocyanurate) | |
| CN105906228A (en) | Method for preparation of cement grinding aid additive from glycerin rectification residue | |
| CN107226569B (en) | Method for treating lithium-containing wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |