CN106362437A - Chromatographic column used for material detection in production apparatus of butyl acrylate - Google Patents
Chromatographic column used for material detection in production apparatus of butyl acrylate Download PDFInfo
- Publication number
- CN106362437A CN106362437A CN201610722771.0A CN201610722771A CN106362437A CN 106362437 A CN106362437 A CN 106362437A CN 201610722771 A CN201610722771 A CN 201610722771A CN 106362437 A CN106362437 A CN 106362437A
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- Prior art keywords
- filler
- chromatographic column
- butyl acrylate
- mass fraction
- carrier
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A chromatographic column used for material detection in production apparatus of butyl acrylate. The invention belongs to the field of detection and analysis of butyl acrylate. An external tube is filled with a mixed filler that is a mixture obtained by uniformly mixing a first filler and a second filler according to the mass ratio of 98.3-99.4:1; a stationary liquid of the first filler is a reaction product of 20M polyethylene glycol and terephthalic acid, mass percentage of the reaction product being 4.8-5.2%, and an H3PO4 acetone solution being 0.48-0.52% in mass percentage; a stationary liquid of the second filler is a reaction product of 20M polyethylene glycol and terephthalic acid, mass percentage of the reaction product being 9.8-10.3%, and an acetone solution of polyneopentyl glycol adipate, of which the mass percentage is 9.8-10.3%. A carrier is a processed white diatomite carrier. The chromatographic column has high accuracy and long service life. The filler is stable and is not liable to lose. The chromatographic column provides accurate and reliable detection data for reducing material loss.
Description
Technical field
The chromatographic column of material detection in a kind of process units for butyl acrylate, belongs to butyl acrylate analysis detection neck
Domain.
Background technology
For the detection of butyl acrylate intermediate products, be generally used at present is the black health chromatographic column that GB uses, but
Shortcoming using black health chromatographic column has: 1, black health chromatographic column, and after a period of time, acrylic acid appearance moves forward, and and acrylic acid
Butyl ester cannot detached problem；2nd, with the increase of use time, same sample data can change, and causes detection data not
Accurately, unstable, usage cycles short it is possible to impact to normal production.
Content of the invention
The technical problem to be solved in the present invention is: overcomes the deficiencies in the prior art, provides one kind to have preferable stability
Chromatographic column with material detection in the reproducible process units for butyl acrylate.
The technical solution adopted for the present invention to solve the technical problems is: this is used for material in butyl acrylate process units
Detection chromatographic column it is characterised in that: be made up of outer tube and filler two parts, outer tube is elongated crimped glass pipe, in outer tube
Be filled with mixed fillers, described mixed fillers be the first filler and the second filler according to mass ratio 98.3 ~ 99.4:1 mixing after
Mixture；The fixative of the wherein first filler is the anti-of 20m Polyethylene Glycol and the p-phthalic acid of mass fraction 4.8% ~ 5.2%
Answer product and the h of mass fraction 0.48% ~ 0.52%3po4Acetone soln；The fixative of the second filler be mass fraction 9.8% ~
10.3% 20m Polyethylene Glycol and the neopentyl glycol adipic acid of the product of p-phthalic acid and mass fraction 9.8% ~ 10.3%
The acetone soln of polyester, the carrier of the carrier of the first filler and the second filler is and processes through overpickling and dimethyldichlorosilane
Phasechrom.
The present invention provides a kind of chromatographic column dedicated for the detection of butyl acrylate process units intermediate material.This chromatographic column
For packing type chromatographic column, add special mixed fillers in outer tube, can accurately detect in butyl acrylate reactor
The present invention is can ensure that after the content of key component, and have preferable stability and repeatability, stability and repeatability are strong
Service life longer, and the present invention successively configures two kinds of fillers, first in the reaction of 20m Polyethylene Glycol and p-phthalic acid
Add a small amount of phosphoric acid in product, then add in the product with p-phthalic acid for the 20m Polyethylene Glycol neopentyl glycol oneself two
Acid polyester, then the filler of two kinds of specific acetone soln states is mixed in proportion, filler has been heightened to acrylic acid and acrylic acid fourth
The sensing sensitivity of ester and diversity, the chromatographic column filler obtaining will not occur " before acrylic acid appearance in use for some time
Move, and cannot separate with butyl acrylate " problem, accuracy is high, long service life, and filler stably not easily runs off, for producing
Device stable and high effective operation, reducing material loss provides accurately and reliably detection data.
Preferably, described outer pipe range 1.8 m ~ 2.2m, internal diameter 0.004 m ~ 0.006m.The length of long 1.8 m ~ 2.2m
Glass tubing crimps as six regular circles, easy to use, and measurement is accurately.
Preferably, the mass ratio of the first described filler and the second filler is 99:1.First filler and the matter of the second filler
, than the most stable of mixed material state that can reach the present invention under this preferred proportion, service life is the longest for amount.
Preferably, the size of the carrier of the described carrier of the first filler and the second filler is 60 ~ 80 mesh.Carrier big
Little main impact specific surface area, the carrier of the present invention can be easier after processing through overpickling and dimethyldichlorosilane and consolidate
Determine liquid to combine and firm absorption, the present invention, after the carrier being defined in this preferred size, can reach optimal mobility, can
Preferably prevent the loss of filler.
The composition of fixative is the technical characteristic of most critical of the present invention, directly determines the accuracy of measurement.Preferably, institute
The fixative of the first filler stated is the 20m Polyethylene Glycol of mass fraction 5% and the product of p-phthalic acid and mass fraction
0.5% h3po4Acetone soln.The fixative of the second described filler is for the 20m Polyethylene Glycol of mass fraction 10% and to benzene
The acetone soln of the neopentyl glycol adipate polyester of the product of dioctyl phthalate and mass fraction 10%.Reach this in fixative excellent
Select the carrier that can preferably adapt to the present invention during condition it is ensured that the measured value of the present invention reach the most accurate, most stable of simultaneously,
Service life is also longer.
The product of described 20m Polyethylene Glycol and p-phthalic acid is 20m Polyethylene Glycol and p-phthalic acid is pressed
The esterification reaction product of the mass ratio of 1:0.3 ~ 4.6.The meaning of 20m Polyethylene Glycol is molecular weight is 20 × 106Poly- second two
Alcohol.
Compared with prior art, the chromatographic column institute that in a kind of process units for butyl acrylate of the present invention, material detects
Have the beneficial effect that the present invention by the adjustment to fixative and carrier, the filled-type chromatographic column obtaining has preferably
Stability and repeatability, dedicated for the detection of butyl acrylate process units intermediate material, are process units stable and high effective operation,
Reducing material loss provides accurately and reliably detection data.Chromatographic column filler stably not easily runs off, long service life, reduces chromatograph
Post renewal cost, saves testing cost.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, and wherein embodiment 1 is optimal embodiment.
Embodiment 1
The outer tube of chromatographic column is long 2.0m, the glass tubing of internal diameter 0.005m, crimps six circles for regular strip；Fill out in outer tube
Dress mixed fillers, mixed fillers are the first filler and the second filler according to the mixture after mass ratio 99:1 mixing；Wherein first
The fixative of filler is the 20m Polyethylene Glycol of mass fraction 5.0% and the product of p-phthalic acid and mass fraction 0.50%
H3po4Acetone soln；The fixative of the second filler is 20m Polyethylene Glycol and the p-phthalic acid of mass fraction 10.0%
The acetone soln of the neopentyl glycol adipate polyester of product and mass fraction 10.0%, the carrier of the first filler and second is filled out
The carrier of material is phasechrom that process, that size is 60 ~ 80 mesh through overpickling and dimethyldichlorosilane.Will
This chromatographic column is installed to and on Shimadzu gc-2014 gas chromatogram instrument, control sample in the middle of butyl acrylate is detected.Detection
Butyl acrylate first reactor material is detected (initial survey 1), and testing result prepares standard after using 12 months with chromatographic column
Sample (standard specimen 1) is verified.
Embodiment 2
The outer tube of chromatographic column is long 1.9m, the glass tubing of internal diameter 0.005m, crimps six circles for regular strip；Fill out in outer tube
Dress mixed fillers, mixed fillers are the first filler and the second filler according to the mixture after mass ratio 98.6:1 mixing；Wherein
The fixative of one filler is the 20m Polyethylene Glycol of mass fraction 4.9% and the product of p-phthalic acid and mass fraction
0.51% h3po4Acetone soln；The fixative of the second filler is 20m Polyethylene Glycol and the terephthaldehyde of mass fraction 10.2%
The acetone soln of the neopentyl glycol adipate polyester of the product of acid and mass fraction 9.9%, the carrier of the first filler and second
The carrier of filler is phasechrom that process, that size is 60 ~ 80 mesh through overpickling and dimethyldichlorosilane.
This chromatographic column is installed on Shimadzu gc-2014 gas chromatogram instrument control sample in the middle of butyl acrylate is detected.Inspection
Survey butyl acrylate first reactor material to be detected (initial survey 2), testing result prepares mark after using 12 months with chromatographic column
Quasi- sample (standard specimen 2) is verified.
Embodiment 3
The outer tube of chromatographic column is long 2.1m, the glass tubing of internal diameter 0.005m, crimps six circles for regular strip；Fill out in outer tube
Dress mixed fillers, mixed fillers are the first filler and the second filler according to the mixture after mass ratio 99.2:1 mixing；Wherein
The fixative of one filler is the 20m Polyethylene Glycol of mass fraction 5.1% and the product of p-phthalic acid and mass fraction
0.49% h3po4Acetone soln；The fixative of the second filler is 20m Polyethylene Glycol and the terephthaldehyde of mass fraction 9.9%
The acetone soln of the neopentyl glycol adipate polyester of the product of acid and mass fraction 10.0%, the carrier of the first filler and the
The carrier of two fillers is white diatomite that process through overpickling and dimethyldichlorosilane, that size is 60 ~ 80 mesh and carries
Body.This chromatographic column is installed on Shimadzu gc-2014 gas chromatogram instrument control sample in the middle of butyl acrylate is detected.
Detection butyl acrylate first reactor material is detected (initial survey 3), and testing result is prepared after being used 12 months with chromatographic column
Standard sample (standard specimen 3) is verified.
Embodiment 4
The outer tube of chromatographic column is long 1.8 m, the glass tubing of internal diameter 0.004 m, crimps six circles for regular strip；In outer tube
Load mixed fillers, mixed fillers are the first filler and the second filler according to the mixture after mass ratio 98.3:1 mixing；Wherein
The fixative of the first filler is the 20m Polyethylene Glycol of mass fraction 4.8% and the product of p-phthalic acid and mass fraction
0.52% h3po4Acetone soln；The fixative of the second filler is 20m Polyethylene Glycol and the terephthaldehyde of mass fraction 9.8%
The acetone soln of the neopentyl glycol adipate polyester of the product of acid and mass fraction 10.3%, the carrier of the first filler and the
The carrier of two fillers is white diatomite that process through overpickling and dimethyldichlorosilane, that size is 60 ~ 80 mesh and carries
Body.This chromatographic column is installed on Shimadzu gc-2014 gas chromatogram instrument control sample in the middle of butyl acrylate is detected.
Detection butyl acrylate first reactor material is detected (initial survey 4), and testing result is prepared after being used 12 months with chromatographic column
Standard sample (standard specimen 4) is verified.
Embodiment 5
The outer tube of chromatographic column is long 2.2m, the glass tubing of internal diameter 0.006m, crimps six circles for regular strip；Fill out in outer tube
Dress mixed fillers, mixed fillers are the first filler and the second filler according to the mixture after mass ratio 99.4:1 mixing；Wherein
The fixative of one filler is the 20m Polyethylene Glycol of mass fraction 5.2% and the product of p-phthalic acid and mass fraction
0.48% h3po4Acetone soln；The fixative of the second filler is 20m Polyethylene Glycol and the terephthaldehyde of mass fraction 10.3%
The acetone soln of the neopentyl glycol adipate polyester of the product of acid and mass fraction 9.8%, the carrier of the first filler and second
The carrier of filler is phasechrom that process, that size is 50 ~ 85 mesh through overpickling and dimethyldichlorosilane.
This chromatographic column is installed on Shimadzu gc-2014 gas chromatogram instrument control sample in the middle of butyl acrylate is detected.Inspection
Survey butyl acrylate first reactor material to be detected (initial survey 5), testing result prepares mark after using 12 months with chromatographic column
Quasi- sample (standard specimen 5) is verified.
Comparative example 1
The outer tube of chromatographic column only fills the first filler of embodiment 1 with embodiment 1, except for the difference that filler, carrier be through overpickling and
Dimethyldichlorosilane is processed, size is the phasechrom of 60 ~ 80 mesh, and this chromatographic column is installed to Shimadzu gc-
On 2014 gas chromatogram instruments, control sample in the middle of butyl acrylate is detected.Detection butyl acrylate first reactor thing
Material is detected (initial survey 6), and testing result is verified using preparation standard sample (standard specimen 6) after 12 months with chromatographic column.
Comparative example 2
, with embodiment 1, except for the difference that carrier is merely through dimethyldichlorosilane process, size for the outer tube of chromatographic column and filler
It is the phasechrom of 60 ~ 80 mesh, this chromatographic column is installed on Shimadzu gc-2014 gas chromatogram instrument to acrylic acid
Sample is controlled to be detected in the middle of butyl ester.Detection butyl acrylate first reactor material is detected (initial survey 7), testing result
Verified using preparation standard sample (standard specimen 7) after 12 months with chromatographic column.
Comparative example 3
The outer tube of chromatographic column and filler with embodiment 1, except for the difference that carrier be merely through pickling processes, size be 60 ~ 80
Purpose phasechrom, this chromatographic column is installed on Shimadzu gc-2014 gas chromatogram instrument in the middle of to butyl acrylate
Sample is controlled to be detected.Detection butyl acrylate first reactor material is detected (initial survey 8), testing result and chromatographic column
Verified using preparing standard sample (standard specimen 8) after 12 months.
The performance test experiment of each embodiment and comparative example, the result of standard specimen and initial survey is the meansigma methodss of six detections, respectively
Control sample and the standard sample prepared in the middle of the same butyl acrylate of chromatograph post detection.
.
The present invention either initial survey or the detection of the standard specimen after 12 months be can be seen that by data above, each group go-on-go surveys knot
Fruit is all accurate, and the use of 12 months does not affect on the separating effect of this chromatographic column and accuracy, and accurately, detection data is steady for data
Fixed.Comparative example can be seen that if when two kinds of fillers do not use jointly in proportion, when carrier is to process as the present invention, color
Although spectrum post early stage can accurately detect, in use for some time, testing result is quite different with reality, and
The data of detection is also stable, comes in and goes out also larger when obtaining meansigma methodss between the result of six detections.
The above, be only presently preferred embodiments of the present invention, is not the restriction that the present invention is made with other forms, appoints
What those skilled in the art possibly also with the disclosure above technology contents changed or be modified as equivalent variations etc.
Effect embodiment.But every without departing from technical solution of the present invention content, according to the present invention technical spirit to above example institute
Any simple modification, equivalent variations and the remodeling made, still falls within the protection domain of technical solution of the present invention.
Claims (6)
1. in a kind of process units for butyl acrylate material detection chromatographic column it is characterised in that: by outer tube and filler two
Part form, outer tube is elongated crimped glass pipe, is filled with mixed fillers in outer tube, described mixed fillers be the first filler and
Second filler is according to the mixture after mass ratio 98.3 ~ 99.4:1 mixing；The fixative of the wherein first filler is mass fraction
4.8% ~ 5.2% 20m Polyethylene Glycol and the h of the product of p-phthalic acid and mass fraction 0.48% ~ 0.52%3po4Third
Ketone solution；The fixative of the second filler is that the 20m Polyethylene Glycol of mass fraction 9.8% ~ 10.3% is produced with the reaction of p-phthalic acid
The acetone soln of the neopentyl glycol adipate polyester of thing and mass fraction 9.8% ~ 10.3%, the carrier of the first filler and the second filler
Carrier be the phasechrom processing through overpickling and dimethyldichlorosilane.
2. the chromatographic column that in a kind of process units for butyl acrylate according to claim 1, material detects, its feature
It is: described outer pipe range 1.8 m ~ 2.2m, internal diameter 0.004 m ~ 0.006m.
3. the chromatographic column that in a kind of process units for butyl acrylate according to claim 1, material detects, its feature
It is: the mass ratio of the first described filler and the second filler is 99:1.
4. the chromatographic column that in a kind of process units for butyl acrylate according to claim 1, material detects, its feature
It is: the size of the carrier of the described carrier of the first filler and the second filler is 60 ~ 80 mesh.
5. the chromatographic column that in a kind of process units for butyl acrylate according to claim 1, material detects, its feature
Be: the fixative of the first described filler be 20m Polyethylene Glycol and the p-phthalic acid of mass fraction 5% product and
The h of mass fraction 0.5%3po4Acetone soln.
6. the chromatographic column that in a kind of process units for butyl acrylate according to claim 1, material detects, its feature
It is: the fixative of the second described filler is the product with p-phthalic acid for the 20m Polyethylene Glycol of mass fraction 10%
Acetone soln with the neopentyl glycol adipate polyester of mass fraction 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610722771.0A CN106362437B (en) | 2016-08-25 | 2016-08-25 | A kind of chromatographic column detected for material in butyl acrylate production device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610722771.0A CN106362437B (en) | 2016-08-25 | 2016-08-25 | A kind of chromatographic column detected for material in butyl acrylate production device |
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| Publication Number | Publication Date |
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| CN106362437A true CN106362437A (en) | 2017-02-01 |
| CN106362437B CN106362437B (en) | 2018-08-03 |
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Citations (4)
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|---|---|---|---|---|
| CN1987453A (en) * | 2005-12-19 | 2007-06-27 | 刘开禄 | High molecular type reverse chromatography fixing phase and its preparing method |
| US20110152499A1 (en) * | 2009-12-21 | 2011-06-23 | Dow Global Technologies Inc. | Chromatography of polyolefin polymers |
| CN103038633A (en) * | 2010-07-08 | 2013-04-10 | 株式会社大赛璐 | Separation/detection column and kit thereof |
| CN104931629A (en) * | 2015-06-19 | 2015-09-23 | 武汉理工大学 | Micro-packed chromatographic column used for measuring total organic pollutant in air and preparation method and use method of micro-packed chromatographic column |
-
2016
- 2016-08-25 CN CN201610722771.0A patent/CN106362437B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1987453A (en) * | 2005-12-19 | 2007-06-27 | 刘开禄 | High molecular type reverse chromatography fixing phase and its preparing method |
| US20110152499A1 (en) * | 2009-12-21 | 2011-06-23 | Dow Global Technologies Inc. | Chromatography of polyolefin polymers |
| CN103038633A (en) * | 2010-07-08 | 2013-04-10 | 株式会社大赛璐 | Separation/detection column and kit thereof |
| CN104931629A (en) * | 2015-06-19 | 2015-09-23 | 武汉理工大学 | Micro-packed chromatographic column used for measuring total organic pollutant in air and preparation method and use method of micro-packed chromatographic column |
Non-Patent Citations (2)
| Title |
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| 刘丹: "顶空气相色谱法测定烟用胶中残余单体", 《分析科学学报》 * |
| 刘薇: "混合单体中丙烯酸丁酯含量的测定", 《贵州化工》 * |
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| CN106362437B (en) | 2018-08-03 |
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