CN106316849B - The method that sensitive impurity extends the shelf life in removal esters reagent - Google Patents
The method that sensitive impurity extends the shelf life in removal esters reagent Download PDFInfo
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- CN106316849B CN106316849B CN201610693378.3A CN201610693378A CN106316849B CN 106316849 B CN106316849 B CN 106316849B CN 201610693378 A CN201610693378 A CN 201610693378A CN 106316849 B CN106316849 B CN 106316849B
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- esters
- esters reagent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to technical field of fine, and in particular to a method of sensitive impurity extends the shelf life in removal esters reagent comprising following steps：(1) esters reagent is flowed through into free stream cataphoresis device, removes the inorganic salt impurities in esters reagent；(2) make esters reagent by alkaline molecular sieve, removing residual acid, moisture and organic impurities；(3) under the conditions of nitrogen protection, esters reagent micro-filtration is handled, then sealed package.Method of the invention is environmentally protective, pollution-free, and treating capacity is big, and treated, and the esters product holding time is long.
Description
Technical field
The invention belongs to technical field of fine, and in particular to sensitive impurity extension is guaranteed the quality in a kind of removal esters reagent
The method of phase.
Background technique
Ester type compound product all contains acid, moisture, small-scale inorganic salt, these impurity because synthesis technology or environment influence
It can make ester-type hydrolysis, and inorganic salts have catalysis efficiency.In addition the moisture in atmospheric environment, oxygen, acidity or alkaline gas meeting
It is dissolved in storage and transportation because sealing deficiency and enters product, can further make ester-type hydrolysis that the impurity such as the acid, water, alcohol of product be caused to contain
Amount increases, the decline of esters quality, to cause that its shelf-life is short, unstable quality.
Storage 1 year or more ester type compound is used in scientific research, analytic process, often to be come by operations such as depickling, rectifying
Purification, causes the waste and environmental pollution of manpower and material resources.It must for this purpose, having very much by the shelf-life that technological progress extends esters product
It wants.
Summary of the invention
Invention broadly provides the method that sensitive impurity in a kind of removal esters reagent extends the shelf life, this method greens
Environmental protection, pollution-free, treating capacity is big, and treated, and the esters product holding time is long.Its technical solution is as follows：A kind of removal esters examination
The method that sensitive impurity extends the shelf life in agent, includes the following steps：
(1) esters reagent is flowed through into free stream cataphoresis device, removes the inorganic salt impurities in esters reagent；
(2) make esters reagent by alkaline molecular sieve, removing residual acid, moisture and organic impurities；
(3) under the conditions of nitrogen protection, esters reagent micro-filtration is handled, then sealed package.
Preferably, the operation voltage of free stream cataphoresis device is 110 ± 5V, operation electric current 1-2A in step (1).
Preferably, step (2) neutral and alkali molecular sieve is 16%KF/NaY：Na-MCM-41：10X=(30-45) wt%：(5-
10) wt%：(50-65) wt%.
Preferably, the mass ratio of step (2) neutral and alkali molecular sieve and esters reagent is 1:(20-50).
Preferably, acidity≤0.0005mmol/g of step (2) treated esters reagent, moisture≤0.05%.
Preferably, micro-filtration processing, tool are carried out to esters reagent using fiber micro-filtration column and the combination of inorganic filter membrane in step (3)
Body, which is elder generation, recycles micro-filtration by 5 μm of fiber micro-filtration column, then through 0.5 μm of inorganic membrane filtration.
The method to be extended the shelf life using impurity sensitive in above-mentioned removal esters reagent, the present invention are had the following advantages that：
The present invention removes inorganic salts (ion) impurity in esters product by free stream cataphoresis, using compound alkaline molecular sieve
Residual acid and moisture are removed simultaneously, micro-filtration is packed under nitrogen atmosphere, to make ester type compound quality that can maintain it before Kaifeng
Outgoing.This method is environmentally protective, pollution-free, and treating capacity is big, it can be achieved that continuous prepare with scale；Another used alkalinity point
Son sieve may be reused after microwave drying, carrying out precipitation treatment.It is found through detection, uses the processed esters reagent 36 of this method
Quality does not change after a month, it follows that esters reagent saves well, the guarantor of esters reagent is conducive to using treatment method
It deposits.
Specific embodiment
Embodiment 1
The method that sensitive impurity extends the shelf life in removal ethyl acetate：
(1) ethyl acetate flows through free stream cataphoresis device (600mm*800mm operates voltage 110V, operation electric current 1A), stream
Fast 1000g per hour collects the treatment fluid of intermediate 50mm-750mm；
(2) 1kg alkaline molecular sieve (16%KF/NaY：Na-MCM-41:10X is 40wt%：5wt%：It 55wt%) is packed into straight
Depickling that diameter is 50mm, dry column, make 45kg ethyl acetate cross column repeatedly, control in product：Acidity≤0.0005mmol/g is (with H+
Meter), moisture≤0.05%；
(3) under nitrogen protection, micro-filtration is successively recycled by 5 μm of fiber micro-filtration column, then through 0.5 μm of inorganic filter membrane mistake
Filter, and then pack and product is made.
Embodiment 2
The method that sensitive impurity extends the shelf life in removal ethyl oxalate：
(1) ethyl oxalate flows through free stream cataphoresis device (600mm*800mm operates voltage 110V, operation electric current 1.5A),
Flow velocity 1000g per hour collects the treatment fluid of intermediate 100mm-700mm；
(2) 1kg alkaline molecular sieve (16%KF/NaY：Na-MCM-41:10X is 40wt%：6wt%：It 54wt%) is packed into straight
Depickling that diameter is 50mm, dry column, make 35kg ethyl oxalate cross column repeatedly, control in product：Acidity≤0.0005mmol/g is (with H+
Meter), moisture≤0.05%；
(3) under nitrogen protection, micro-filtration is successively recycled by 5 μm of fiber micro-filtration column, then through 0.5 μm of inorganic filter membrane mistake
Filter, and then pack and product is made.
Embodiment 3
The method that sensitive impurity extends the shelf life in removal triacetyl glycerine：
(1) triacetyl glycerine flows through free stream cataphoresis device (600mm*800mm, operation voltage 110V, operation electric current
2A), flow velocity 1000g per hour collects the treatment fluid of intermediate 100mm-700mm；
(2) 1kg alkaline molecular sieve (16%KF/NaY：Na-MCM-41:10X is 45wt%：5wt%：It 50wt%) is packed into straight
Depickling that diameter is 50mm, dry column, make 30kg triacetyl glycerine cross column repeatedly, control in product：Acidity≤0.0005mmol/g
(in terms of H+), moisture≤0.05%；
(3) under nitrogen protection, micro-filtration is successively recycled by 5 μm of fiber micro-filtration column, then through 0.5 μm of inorganic filter membrane mistake
Filter, and then pack and product is made.
Experimental result detection
Before dispatching from the factory to the processed esters reagent of embodiment 1-3,12 months, moisture, acidity and quality after 36 months
The detection of content, and be respectively control with not processed esters reagent, testing result is as shown in table 1：
1 esters reagent of table saves testing result
By testing result it is found that for ethyl acetate, 36 months guarantors are passed through through treated the ethyl acetate of embodiment 1
It deposits, front and back moisture, acidity and mass content are without significant change, and commercially available ethyl acetate has not behind 12 months and 36 months
With the variation of degree.For ethyl oxalate, through treated ethyl oxalate the passes through preservation in 36 months of embodiment 2, front and back moisture,
Acidity and mass content are without significant change, and commercially available ethyl oxalate has different degrees of change behind 12 months and 36 months
Change.For triacetyl glycerine, through treated triacetyl glycerine passes through preservation in 36 months, the front and back moisture, acid of embodiment 3
Degree and mass content are without significant change, and commercially available triacetyl glycerine has different degrees of change behind 12 months and 36 months
Change.It follows that the processing method of embodiment 1-3 is conducive to the long-term preservation of esters reagent.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (6)
1. a kind of method that sensitive impurity extends the shelf life in removal esters reagent, it is characterised in that：Include the following steps：
(1) esters reagent is flowed through into free stream cataphoresis device, removes the inorganic salt impurities in esters reagent；
(2) make esters reagent by alkaline molecular sieve, removing residual acid, moisture and organic impurities；
(3) under the conditions of nitrogen protection, esters reagent micro-filtration is handled, then sealed package.
2. the method that sensitive impurity extends the shelf life in removal esters reagent according to claim 1, it is characterised in that：Step
Suddenly the operation voltage of free stream cataphoresis device is 110 ± 5V, operation electric current 1-2A in (1).
3. the method that sensitive impurity extends the shelf life in removal esters reagent according to claim 1, it is characterised in that：Step
Suddenly (2) neutral and alkali molecular sieve is 16%KF/NaY：Na-MCM-41：10X=(30-45) wt%：(5-10) wt%：(50-65)
Wt%.
4. the method that sensitive impurity extends the shelf life in removal esters reagent according to claim 1, it is characterised in that：Step
Suddenly the mass ratio of (2) neutral and alkali molecular sieve and esters reagent is 1:(20-50).
5. the method that sensitive impurity extends the shelf life in removal esters reagent according to claim 1, it is characterised in that：Step
Suddenly acidity≤0.0005mmol/g of (2) treated esters reagent, moisture≤0.05%.
6. the method that sensitive impurity extends the shelf life in removal esters reagent according to claim 1, it is characterised in that：Step
Suddenly micro-filtration processing method is first to recycle micro-filtration by 5 μm of fiber micro-filtration column in (3), then through 0.5 μm of inorganic membrane filtration.
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| CN201610693378.3A CN106316849B (en) | 2016-08-18 | 2016-08-18 | The method that sensitive impurity extends the shelf life in removal esters reagent |
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| CN106316849B true CN106316849B (en) | 2018-11-23 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4020966A1 (en) * | 1990-06-30 | 1992-01-16 | Hoechst Ag | Detection of sulphated oligo- and polysaccharide(s) - using poly base, and methylene blue opt. with an oxidising agent or auramine |
| CN104693028A (en) * | 2015-03-31 | 2015-06-10 | 太仓沪试试剂有限公司 | Purification method of ethyl acetate |
| CN105622415A (en) * | 2016-02-18 | 2016-06-01 | 国药集团化学试剂有限公司 | Ethyl acetate quality improving method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1404643A4 (en) * | 2001-05-29 | 2008-05-07 | Univ Vanderbilt | Cleavable surfactants and methods of use thereof |
| KR100862236B1 (en) * | 2006-11-22 | 2008-10-09 | (주)엘에스티코리아 | 1,1'-oxalyldisodiumbenzoate derivates, preparing method thereof and chemiluminescent composition containing the same |
-
2016
- 2016-08-18 CN CN201610693378.3A patent/CN106316849B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4020966A1 (en) * | 1990-06-30 | 1992-01-16 | Hoechst Ag | Detection of sulphated oligo- and polysaccharide(s) - using poly base, and methylene blue opt. with an oxidising agent or auramine |
| CN104693028A (en) * | 2015-03-31 | 2015-06-10 | 太仓沪试试剂有限公司 | Purification method of ethyl acetate |
| CN105622415A (en) * | 2016-02-18 | 2016-06-01 | 国药集团化学试剂有限公司 | Ethyl acetate quality improving method |
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| CN106316849A (en) | 2017-01-11 |
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