CN106517247A - Method for preparing high-purity sodium chloride by refining alkyl-capped polyether byproduct salt - Google Patents
Method for preparing high-purity sodium chloride by refining alkyl-capped polyether byproduct salt Download PDFInfo
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- CN106517247A CN106517247A CN201610597587.8A CN201610597587A CN106517247A CN 106517247 A CN106517247 A CN 106517247A CN 201610597587 A CN201610597587 A CN 201610597587A CN 106517247 A CN106517247 A CN 106517247A
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- capped polyether
- sodium chloride
- purity sodium
- product salt
- alkyl
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- 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
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Life Sciences & Earth Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Polyethers (AREA)
Abstract
The invention provides a method for preparing high-purity sodium chloride by refining an alkyl-capped polyether byproduct salt. The method comprises the following steps: dissolving the capped polyether byproduct salt in water according to a certain proportion, and adjusting the pH value of an aqueous solution by using acid; adding an organic solvent to extract an organic matter in a water phase; performing standing for demixing and liquid separation; removing the solvent with an organic phase, and then recovering capped polyether; and performing evaporative crystallization on the water phase to prepare high-purity sodium chloride. According to the method provided by the invention, the high-purity sodium chloride is prepared by refining salt residues of alkyl-capped polyether, and meanwhile the capped polyether in the salt residues is recovered, thereby achieving green production of the capped polyether.
Description
Technical field
The invention belongs to end capped polyether technical field, and in particular to a kind of refinement treatment work of alkyl capped polyether by-product salt
Skill.
Background technology
The general structure of alkyl capped polyether：
The synthesis of alkyl capped polyether generally adopts wiliamosn synthetic methods, and preparing generally point 3 steps is carried out：(1) monoalkyl polyoxy
Ethene, polyoxypropylene（Or polybutylene）Ether（It is block, random）Preparation；(2) the preparation of monoalkyl polyethers sodium thing；(3) block
The synthesis of polyethers.
Industrially, in order to improve the ending ratio of polyethers, often using excessive sodium alkoxide, this causes alkyl capped polyether by-product
Salt slag in addition to containing the organic matter such as end capped polyether and sodium chloride, also containing substantial amounts of NaOH, be difficult to without process
Recycle, cause the waste of resource and the pollution of environment.
Patent CN201110407580.2 reports a kind of alkyl-blocked finishing process method of PPOX, polycyclic
After the completion of the reaction of Ethylene Oxide end capped polyether, the salt in system is dissolved with water, and separated with organic matter, then the absorption of Jing adsorbents,
Reduced pressure concentration, crystallisation by cooling prepare refined sodium chloride.Using inevitably containing hydrogen in the sodium chloride product that the method is obtained
Sodium oxide molybdena, affects the purity and use range of sodium chloride.
Patent CN200910029891.2 describes a kind of method that employing high-temperature calcination processes end capped polyether by-product salt slag,
The method needs the organic matters such as the remaining end capped polyether in calcining and decomposing end capped polyether by-product salt at 400 ~ 600 DEG C, wastes money
Source, is unfavorable for environmental protection.
The content of the invention
It is an object of the invention to provide a kind of method from alkyl capped polyether by-product salt refining high-purity sodium chloride, the party
Method has reclaimed the end capped polyether in salt slag, and obtains highly purified sodium chloride product, reduces the waste of resource.
In order to reach object above, the present invention provides following technical scheme：
A kind of method that alkyl capped polyether by-product salt refining prepares high-purity sodium chloride, comprises the following steps：
(1). by adding water, stirring and dissolving in the salt slag to end capped polyether by-product；
(2). acid is added in solution, adjusts pH；
(3). extractant, extraction stratification is added in solution；
(4). mutually divide liquid to the organic phase on upper strata with the water of lower floor；
(5). organic phase desolvation reclaims end capped polyether product；
(6). water phase evaporative crystallization, filters, obtains high-purity sodium chloride.
Preferably, the weight of the step (1) water of middle addition is 2.5 ~ 3.2 times of end capped polyether by-product salt slag weight.
Preferably, step (2) in for adjust solution ph acid be hydrochloric acid.
Preferably, the pH value of step solution (2) after middle regulation is 6 ~ 8.
Preferably, step (3) described in extractant be n-hexane, hexamethylene, ethyl acetate, the one kind or many in toluene
The mixed solvent planted.
Preferably, step (3) described in extractant consumption for end capped polyether by-product salt slag weight 30% ~ 50%.
Preferably, step (5) middle organic phase desolvation method be reduced pressure concentration.
Preferably, step (6) described in evaporative crystallization be that air-distillation or vacuum distillation are dehydrated.
Preferably, step (6) described in evaporative crystallization, steam moisture weight be alkyl capped polyether by-product salt weight
1.8 ~ 2.5 times.
What the present invention was obtained has the beneficial effect that：
The method that the present invention is provided has reclaimed the end capped polyether in salt slag, and obtains highly purified sodium chloride product, reduces
The waste of resource.The problems such as salt slag produced in solving alkyl capped polyether production process cannot be recycled, pollute environment.
The processing method technological operation that the present invention is provided simply easily is implemented, and gained sodium chloride high purity more than 99.5% reaches refined work
The requirement of industry salt one-level.
Specific embodiment
With reference to specific embodiment, the present invention is further elucidated, it should be understood that following specific embodiments are only used for
The bright present invention rather than restriction the scope of the present invention.
Embodiment 1
10kg alkyl capped polyether by-product salt is weighed, 30kg water is added, with salt acid for adjusting pH to 7.0 after stirring and dissolving, is just added
Hexane 3kg, extraction stratification, then mutually divide liquid to the organic phase on upper strata with the water of lower floor, make organic phase and aqueous phase separation.
Organic phase carries out reduced pressure concentration at 40 DEG C, and recovery obtains end capped polyether 1.02kg and n-hexane 2.95kg.
Water phase evaporative crystallization, filters to obtain high-purity sodium chloride, and Jing is determined, and sodium chloride content is 99.8%.
Embodiment 2
10kg alkyl capped polyether by-product salt is weighed, 28kg water is added, with salt acid for adjusting pH to 7.0 after stirring and dissolving, second is added
Acetoacetic ester 5kg, extraction stratification, then mutually divide liquid to the organic phase on upper strata with the water of lower floor, organic phase is mutually divided with water
From.
Organic phase carries out reduced pressure concentration at 40 DEG C, and recovery obtains end capped polyether 1.04kg and ethyl acetate 4.93kg.
Water phase evaporative crystallization, filters to obtain high-purity sodium chloride, and Jing is determined, and sodium chloride content is 99.6%.
Embodiment 3
10kg alkyl capped polyether by-product salt is weighed, 25kg water is added, with salt acid for adjusting pH to 6.0 after stirring and dissolving, first is added
Benzene 4kg, extraction stratification, then mutually divide liquid to the organic phase on upper strata with the water of lower floor, make organic phase and aqueous phase separation.
Organic phase carries out reduced pressure concentration at 45 DEG C, and recovery obtains end capped polyether 1.03kg and toluene 3.94kg.
Water phase evaporative crystallization, filters to obtain high-purity sodium chloride, and Jing is determined, and sodium chloride content is 99.5%.
Embodiment 4
10kg alkyl capped polyether by-product salt is weighed, 32kg water is added, with salt acid for adjusting pH to 8.0 after stirring and dissolving, ring is added
Hexane 3kg, extraction stratification, then mutually divide liquid to the organic phase on upper strata with the water of lower floor, make organic phase and aqueous phase separation.
Organic phase carries out reduced pressure concentration at 35 DEG C, and recovery obtains end capped polyether 1.04kg and hexamethylene 2.94kg.
Water phase evaporative crystallization, filters to obtain high-purity sodium chloride, and Jing is determined, and sodium chloride content is 99.7%.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned embodiment, also includes
Constituted technical scheme is combined by above technical characteristic.It should be pointed out that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (9)
1. a kind of method that alkyl capped polyether by-product salt refining prepares high-purity sodium chloride, it is characterised in that including following step
Suddenly：
(1). by adding water, stirring and dissolving in the salt slag to end capped polyether by-product；
(2). acid is added in solution, adjusts pH；
(3). extractant, extraction stratification is added in solution；
(4). mutually divide liquid to the organic phase on upper strata with the water of lower floor；
(5). organic phase desolvation reclaims end capped polyether product；
(6). water phase evaporative crystallization, filters, obtains high-purity sodium chloride.
2. the method that alkyl capped polyether by-product salt refining as claimed in claim 1 prepares high-purity sodium chloride, its feature exist
In the weight of, the step (1) water of middle addition be 2.5 ~ 3.2 times of end capped polyether by-product salt slag weight.
3. the method that alkyl capped polyether by-product salt refining as claimed in claim 1 prepares high-purity sodium chloride, its feature exist
In, step (2) in be hydrochloric acid for the acid that adjusts solution ph.
4. the method that the alkyl capped polyether by-product salt refining as described in claim 1 or 3 prepares high-purity sodium chloride, its feature
It is that the pH value of step solution (2) after middle regulation is 6 ~ 8.
5. the method that alkyl capped polyether by-product salt refining as claimed in claim 1 prepares high-purity sodium chloride, its feature exist
In, step (3) described in extractant be n-hexane, hexamethylene, ethyl acetate, one or more in toluene of mixed solvent.
6. the method that the alkyl capped polyether by-product salt refining as described in claim 1 or 5 prepares high-purity sodium chloride, its feature
Be, step (3) described in extractant consumption for end capped polyether by-product salt slag weight 30% ~ 50%.
7. the method that alkyl capped polyether by-product salt refining as claimed in claim 1 prepares high-purity sodium chloride, its feature exist
In the method for, step (5) middle organic phase desolvation be reduced pressure concentration.
8. the method that alkyl capped polyether by-product salt refining as claimed in claim 1 prepares high-purity sodium chloride, its feature exist
In, step (6) described in evaporative crystallization be that air-distillation or vacuum distillation are dehydrated.
9. the method that the alkyl capped polyether by-product salt refining as described in claim 1 or 8 prepares high-purity sodium chloride, its feature
Be, step (6) described in evaporative crystallization, steam the weight of moisture for 1.8 ~ 2.5 times of alkyl capped polyether by-product salt weight.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610597587.8A CN106517247A (en) | 2016-07-27 | 2016-07-27 | Method for preparing high-purity sodium chloride by refining alkyl-capped polyether byproduct salt |
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| CN201610597587.8A CN106517247A (en) | 2016-07-27 | 2016-07-27 | Method for preparing high-purity sodium chloride by refining alkyl-capped polyether byproduct salt |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455741A (en) * | 2018-11-29 | 2019-03-12 | 华南理工大学 | A kind of low-temperature bake and interface regulate and control the method that method recycling complete utilization sodium chloride waste salt dregs are used in conjunction |
| CN109570194A (en) * | 2018-11-23 | 2019-04-05 | 华南理工大学 | A kind of full recycling processing method of sodium sulfate salt slag |
| CN111453907A (en) * | 2020-04-08 | 2020-07-28 | 大连百傲化学股份有限公司 | Recycling treatment process of waste brine in production of 1, 2-benzisothiazolin-3-one |
Citations (5)
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| JPS4914841B1 (en) * | 1970-12-19 | 1974-04-10 | ||
| US4587365A (en) * | 1984-10-29 | 1986-05-06 | Basf Corporation | Preparing capped polyoxyalkylene polyols |
| CN101445434A (en) * | 2008-12-30 | 2009-06-03 | 浙江合诚化学有限公司 | Synthetic method of methyl-terminated polyether |
| CN101670250A (en) * | 2008-09-12 | 2010-03-17 | 中国科学院理化技术研究所 | Alkyl-terminated alkylphenol polyoxyethylene ether benzene sulfonate surfactant and preparation method and application thereof |
| CN102516524A (en) * | 2011-12-09 | 2012-06-27 | 南京威尔化工有限公司 | Post-treatment process method of alkyl blocking of poly(propylene oxide) |
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2016
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| JPS4914841B1 (en) * | 1970-12-19 | 1974-04-10 | ||
| US4587365A (en) * | 1984-10-29 | 1986-05-06 | Basf Corporation | Preparing capped polyoxyalkylene polyols |
| CN101670250A (en) * | 2008-09-12 | 2010-03-17 | 中国科学院理化技术研究所 | Alkyl-terminated alkylphenol polyoxyethylene ether benzene sulfonate surfactant and preparation method and application thereof |
| CN101445434A (en) * | 2008-12-30 | 2009-06-03 | 浙江合诚化学有限公司 | Synthetic method of methyl-terminated polyether |
| CN102516524A (en) * | 2011-12-09 | 2012-06-27 | 南京威尔化工有限公司 | Post-treatment process method of alkyl blocking of poly(propylene oxide) |
Non-Patent Citations (1)
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| 毛培坤等: ""双烷基聚氧烷烯醚的合成"", 《无锡轻工业学院学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109570194A (en) * | 2018-11-23 | 2019-04-05 | 华南理工大学 | A kind of full recycling processing method of sodium sulfate salt slag |
| CN109570194B (en) * | 2018-11-23 | 2022-03-29 | 华南理工大学 | Full recycling treatment method of sodium sulfate slag |
| CN109455741A (en) * | 2018-11-29 | 2019-03-12 | 华南理工大学 | A kind of low-temperature bake and interface regulate and control the method that method recycling complete utilization sodium chloride waste salt dregs are used in conjunction |
| 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 |
| CN111453907A (en) * | 2020-04-08 | 2020-07-28 | 大连百傲化学股份有限公司 | Recycling treatment process of waste brine in production of 1, 2-benzisothiazolin-3-one |
| CN111453907B (en) * | 2020-04-08 | 2022-03-08 | 大连百傲化学股份有限公司 | Recycling treatment process of waste brine in production of 1, 2-benzisothiazolin-3-one |
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Address after: 210047, No. 99 Hexi Road, Nanjing chemical industry park, Jiangsu, Nanjing Applicant after: Nanjing Weier pharmaceutical Limited by Share Ltd Address before: 210047, No. 99 Hexi Road, Nanjing chemical industry park, Jiangsu, Nanjing Applicant before: Weier Chemical Co., Ltd., Nanjing |
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Application publication date: 20170322 |
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