CN109975289A - A kind of rapid detection method of n-butyl acrylate polymer - Google Patents
A kind of rapid detection method of n-butyl acrylate polymer Download PDFInfo
- Publication number
- CN109975289A CN109975289A CN201910316759.3A CN201910316759A CN109975289A CN 109975289 A CN109975289 A CN 109975289A CN 201910316759 A CN201910316759 A CN 201910316759A CN 109975289 A CN109975289 A CN 109975289A
- Authority
- CN
- China
- Prior art keywords
- butyl acrylate
- methanol
- rapid detection
- detection method
- acrylate polymer
- 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.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of rapid detection methods of n-butyl acrylate polymer, and n-butyl acrylate and methanol solution are weighed respectively by weight and are placed in tool plug glass colorimetric cylinder, after rocking under constant temperature conditions uniformly, stands and observes.Rapid detection method provided by the invention greatly shortens detection time, simplifies detecting step, and testing cost is low, testing result is accurate and reliable.
Description
Technical field
The present invention relates to quick detection more particularly to a kind of rapid detection methods of n-butyl acrylate polymer.
Background technique
N-butyl acrylate is mainly used for synthetic resin, synthetic fibers, synthetic rubber, plastics, coating, adhesive etc., also
It may be used as the monomer and its organic synthesis intermediate of polymer and resin.
N-butyl acrylate chemical property is active, and is inflammable and explosive and volatile liquid at normal temperature, because of its carbonyl Q
There is unsaturated double bond structure with B location, easily polymerize under certain conditions, forms a kind of porous insoluble, volume
Loose " end group " polymer, during the production of n-butyl acrylate and storage, especially rectification and purification when, because having temperature
The features such as degree is high, state in which is vapour phase and liquid phase coexists, concentration is high, these factors are all easily cause popcorn polymer positive
Condition, therefore often end occurs and polymerize with condenser top in rectifying column, pipeline blockage is caused, influences normally to produce.It is storing up
It when depositing, once having a certain condition of polymerization, just will appear polymerism, cause pipeline blockage, or even entire storage tank large area
Polymerization, causes great economic loss, or even lead to considerable safety event.N-butyl acrylate polymerization reaction is characterized in: because
Accidentalia causes,, also can shape even if a few hours are interior at low temperature once occurring rapidly to increase using starting polymer as core
At big bulk polymer.
Therefore rotten for discovery n-butyl acrylate polymerization early, it avoids using the positive fourth of the acrylic acid containing number of polymers
Ester production causes scrap of the product even to lead to safety accident, needs to research and develop a kind of side of quickly detection n-butyl acrylate polymer
Method quickly judges whether n-butyl acrylate polymerize, takes precautions against the production-induced production loss of unqualified material and peace in advance
Full hidden danger is fallen.
Summary of the invention
The present invention provides a kind of rapid detection method of n-butyl acrylate polymer, quickly judges that n-butyl acrylate is poly-
Close whether object exceeds manufacturing technique requirent, save detection time and cost, production loss caused by effectively avoiding because of polymer and
Security risk.
Technical solution provided by the present invention is as follows:
A kind of rapid detection method of n-butyl acrylate polymer, by n-butyl acrylate and methanol solution by weight respectively
It weighs and is placed in tool plug glass colorimetric cylinder, after rocking under constant temperature conditions uniformly, stand observation.
Since n-butyl acrylate and its polymer are completely soluble in methanol, but n-butyl acrylate polymer is in first
Solubility in alcoholic solution reduces, and n-butyl acrylate can be completely dissolved in methanol solution, and the present invention is utilizing acrylic acid just
Butyl ester and n-butyl acrylate polymer press n-butyl acrylate to be measured and methanol solution in the difference of methanol solution solubility
Weight ratio is placed in constant temperature mixing in tool plug glass colorimetric cylinder, and the n-butyl acrylate polymer that can not be dissolved becomes cloudy solution,
It then can quickly judge whether n-butyl acrylate occurs polymerization and generate polymer by observing the turbidity of solution, and use tool plug glass
Glass colorimetric cylinder can guarantee that in mixed process be not in solution water clock as mixing vessel, and the container of glass material is more easily saturating
Turbidity depending on observing internal solution reduces judgement of the container to measurement result, generally fills in glass colorimetric cylinder using 50ml tool,
It can be used and use glass tube as test container than turbid.Vertically same in darkroom umbrella canopy lamp can be placed in after mixing under constant temperature conditions
Under, the observation judgement from horizontal direction under conditions of illumination is 1000lx.Rapid detection method operating procedure provided by the invention
Few, without adding chemical reagent reaction, testing cost is low, and detection speed is fast, and testing result can be obtained directly by range estimation, examines
It surveys high-efficient.
Further, the configuration method of the methanol solution is that methanol and distilled water is taken to mix by weight the ratio of 7:3.
The methanol solution being prepared in this ratio can effectively dissolve n-butyl acrylate, and n-butyl acrylate polymer does not dissolve in this
The methanol solution of ratio, so as to whether muddy judge whether n-butyl acrylate generates polymerization by observation methanol solution
Object.
Further, the methanol is anhydrous methanol, moisture≤0.05%.It prepares to guarantee to prepare using anhydrous methanol and obtain
Methanol solution can sufficiently dissolve n-butyl acrylate and insoluble n-butyl acrylate polymer.
Further, the n-butyl acrylate and methanol solution are 2:3~3:4 by weight mixed proportion.Acrylic acid
N-butyl and methanol solution are mixed according to this ratio can guarantee that n-butyl acrylate is dissolved completely in methanol solution and acrylic acid
N-butyl polymer judges insoluble in quickly detection in methanol solution, is conducive to.
Further, the constant temperature is constant temperature water bath, and thermostat temperature is 24 DEG C~26 DEG C, described a length of 1 when rocking
~2 minutes.Under the conditions of this thermostat temperature, n-butyl acrylate, which can be completely dissolved, can't occur polymerization reaction, and acrylic acid is just
Butyl ester polymer is insoluble to make solution muddiness occur, and polymerization reaction is easy to happen if temperature is higher than 26 DEG C influences result judgement, and
Cause solution to become clarification with the solubility increase that temperature increases polymer, influences the accuracy of result judgement；Temperature is lower than 24 DEG C
The solubility for influencing n-butyl acrylate, is easy to cause testing result to judge by accident, it is complete to rock 1~2 minute guarantee n-butyl acrylate
Fully dissolved, polymer disperses polymer in the solution by rocking if it exists, facilitates observation.
It is provided by the invention to have the beneficial effect that:
The first, detection efficiency is high；The present invention utilizes n-butyl acrylate under the conditions of 24 DEG C~26 DEG C of constant temperature to dissolve in methanol: water
The methanol solution of=7:3, and the physical property that n-butyl acrylate is insoluble, in proportion mix n-butyl acrylate and methanol solution
It closes, can determine whether to generate n-butyl acrylate polymer by the turbidity of visual observations solution, and operating procedure is simple,
Detection efficiency is high, greatly shortens material detection time before production；
The second, testing cost is low；The present invention using n-butyl acrylate and its polymer methanol solution different solubility into
Row polymer quickly detects, and without adding other chemical reagent assisted reactions, testing cost is low；
Third, accuracy in detection are high；The present invention using n-butyl acrylate and its polymer in methanol solution in different solubility,
By observation solution whether muddiness judges whether containing polymer, if n-butyl acrylate be dissolved in methanol solution formed it is clear
Solution, then for being not in the problem of pipeline blockage causes production to terminate, accuracy in detection height when producing；
4th, production loss is effectively reduced；Since the aggregation of n-butyl acrylate polymer is easy to cause pipeline in production process
Blocking, causes great economic loss, or even lead to serious accident, can be thrown in production using rapid detection method of the present invention
Quickly whether detection n-butyl acrylate generates n-butyl acrylate polymer during storage before material, and quickly can judgement be used
In production, production loss is effectively reduced.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
The invention discloses a kind of rapid detection methods of n-butyl acrylate polymer, by n-butyl acrylate and methanol
Solution weighs respectively by weight to be placed in tool plug glass colorimetric cylinder, after rocking under constant temperature conditions uniformly, is stood and is observed
Wherein, the configuration method of the methanol solution is that methanol and distilled water is taken to mix by weight the ratio of 7:3.
Wherein, the methanol is anhydrous methanol, moisture≤0.05%.
Wherein, the n-butyl acrylate and methanol solution are 2:3~3:4 by weight mixed proportion.
Wherein, the constant temperature is constant temperature water bath, and thermostat temperature is 24 DEG C~26 DEG C, described 1~2 point a length of when rocking
Clock.
Below by way of specific embodiment, the present invention will be described in detail.It should be appreciated that these embodiments be only it is exemplary,
It does not constitute a limitation on the scope of protection of the present invention.
Embodiment 1
Methanol and distilled water that water content is 0.03% is taken to be mixed to get methanol solution by weight the ratio of 7:3；Ratio by weight
2:3 weighs n-butyl acrylate (lot number: B19116) sample respectively and methanol solution is placed in 50ml tool plug glass colorimetric cylinder, sets
It stands and is immediately placed under umbrella canopy lamp after being shaken 1 minute under the conditions of 25 DEG C in water-bath shaking machine, muddy, judgement occurs in solution
This batch contains n-butyl acrylate polymer, does not meet production requirement.
Embodiment 2
Methanol and distilled water that water content is 0.05% is taken to be mixed to get methanol solution by weight the ratio of 7:3；Ratio by weight
3:4 weighs n-butyl acrylate (lot number: B19208) sample respectively and methanol solution is placed in 50ml tool plug glass colorimetric cylinder, sets
It stands and is immediately placed under umbrella canopy lamp after being shaken 1 minute under the conditions of 26 DEG C in water-bath shaking machine, solution clarification judges this batch
The secondary n-butyl acrylate polymer without the production that has an impact, meets production requirement.
Embodiment 3
Methanol and distilled water that water content is 0.04% is taken to be mixed to get methanol solution by weight the ratio of 7:3；Ratio by weight
7:10 weighs n-butyl acrylate (lot number: B19018) sample respectively and methanol solution is placed in 50ml tool plug glass colorimetric cylinder,
It is placed in water-bath shaking machine after shaking 2 minutes under the conditions of 25 DEG C to stand and be immediately placed under umbrella canopy lamp and observe, solution occurs muddy
It is turbid, judge that this batch contains the n-butyl acrylate polymer for the production that has an impact, does not meet production requirement.
Embodiment 4
Methanol and distilled water that water content is 0.05% is taken to be mixed to get methanol solution by weight the ratio of 7:3；Ratio by weight
2:3 weighs n-butyl acrylate (lot number: B19103) sample respectively and methanol solution is placed in 50ml tool plug glass colorimetric cylinder, sets
It stands and is immediately placed under umbrella canopy lamp after being shaken 2 minutes under the conditions of 25 DEG C in water-bath shaking machine and observed, solution clarification, judgement
This batch is free of the n-butyl acrylate polymer for the production that has an impact, and meets production requirement.
The reason of causing n-butyl acrylate polymerization be it is various, main cause is related with its own property, because third
Olefin(e) acid N-butyl carbonyl Q and B location have unsaturated double bond structure, are inclined to high polymerization, are also easy to produce free electron, and one
Denier generates free electron, will generate an activated centre because of the movement of electronics to cause polymerization, n-butyl acrylate gathers
Closing reaction is exothermic reaction, and the heat generated during polymerization will lead to the further occurrence and aggravation of polymerization, finally make
Production run is terminated because of polymerization.Therefore production caused by the polymerization reaction with n-butyl acrylate terminates as judgment criteria, point
The n-butyl acrylate detected of above-described embodiment 1 to 4 is not taken to carry out small-scale production respectively, wherein embodiment 1 and embodiment 3
N-butyl acrylate occur large area polymerization and blocking pipeline, and the third of embodiment 2 and embodiment 4 in production reaction process
Olefin(e) acid N-butyl does not occur the phenomenon that polymerization blocking pipeline in producing reaction process, it was demonstrated that n-butyl acrylate of the present invention
The rapid detection method measurement result of polymer is reliable.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form；It is all
The those of ordinary skill of the industry can implement the present invention by the above and swimmingly；But all technologies for being familiar with this profession
Personnel without departing from the scope of the present invention, a little change for being made using disclosed above technology contents,
Modification and the equivalent variations developed, are equivalent embodiment of the invention；Meanwhile all substantial technologicals according to the present invention are to above
The variation, modification and evolution etc. of any equivalent variations made by embodiment still fall within the protection model of technical solution of the present invention
Within enclosing.
Claims (5)
1. a kind of rapid detection method of n-butyl acrylate polymer, it is characterised in that: n-butyl acrylate and methanol is molten
Liquid weighs respectively by weight to be placed in tool plug glass colorimetric cylinder, after rocking under constant temperature conditions uniformly, is stood and is observed.
2. the rapid detection method of n-butyl acrylate polymer according to claim 1, it is characterised in that: the methanol
The configuration method of solution is that methanol and distilled water is taken to mix by weight the ratio of 7:3.
3. the rapid detection method of n-butyl acrylate polymer according to claim 2, it is characterised in that: the methanol
For anhydrous methanol, moisture≤0.05%.
4. the rapid detection method of n-butyl acrylate polymer according to claim 1, it is characterised in that: the propylene
Sour N-butyl and methanol solution are 2:3~3:4 by weight mixed proportion.
5. the rapid detection method of n-butyl acrylate polymer according to any one of claims 1 to 4, feature exist
It is constant temperature water bath in: the constant temperature, thermostat temperature is 24 DEG C~26 DEG C, described 1~2 minute a length of when rocking.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910316759.3A CN109975289A (en) | 2019-04-19 | 2019-04-19 | A kind of rapid detection method of n-butyl acrylate polymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910316759.3A CN109975289A (en) | 2019-04-19 | 2019-04-19 | A kind of rapid detection method of n-butyl acrylate polymer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109975289A true CN109975289A (en) | 2019-07-05 |
Family
ID=67085416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910316759.3A Pending CN109975289A (en) | 2019-04-19 | 2019-04-19 | A kind of rapid detection method of n-butyl acrylate polymer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109975289A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050234261A1 (en) * | 2004-04-14 | 2005-10-20 | Honeywell International Inc. | Process for preparing cinnamic acids and alkyl esters thereof |
| CN102173990A (en) * | 2011-03-16 | 2011-09-07 | 抚州市嘉临化工助剂厂 | Preparation method of butyl acrylate |
| CN103454355A (en) * | 2013-08-28 | 2013-12-18 | 天津爱勒易医药材料有限公司 | Method for analyzing and detecting content of monomer in polyacrylic resin latex solution (enteric type) product |
| CN105044234A (en) * | 2015-07-03 | 2015-11-11 | 中华人民共和国台州出入境检验检疫局 | Method for detecting specific migration amounts of thirteen methacrylic acids/esters in plastic product |
-
2019
- 2019-04-19 CN CN201910316759.3A patent/CN109975289A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050234261A1 (en) * | 2004-04-14 | 2005-10-20 | Honeywell International Inc. | Process for preparing cinnamic acids and alkyl esters thereof |
| CN102173990A (en) * | 2011-03-16 | 2011-09-07 | 抚州市嘉临化工助剂厂 | Preparation method of butyl acrylate |
| CN103454355A (en) * | 2013-08-28 | 2013-12-18 | 天津爱勒易医药材料有限公司 | Method for analyzing and detecting content of monomer in polyacrylic resin latex solution (enteric type) product |
| CN105044234A (en) * | 2015-07-03 | 2015-11-11 | 中华人民共和国台州出入境检验检疫局 | Method for detecting specific migration amounts of thirteen methacrylic acids/esters in plastic product |
Non-Patent Citations (1)
| Title |
|---|
| 高筠 等: "甲基丙烯酸丁酯微乳液聚合", 《河北理工学院学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20170029670A1 (en) | Polyolefin based hot melt adhesive composition | |
| CN106255720A (en) | Multilayer film random propylene-ethylene copolymers | |
| CN109975289A (en) | A kind of rapid detection method of n-butyl acrylate polymer | |
| CN107189002A (en) | Chemical modification prepares itself tool defoaming function polyvinyl alcohol and preparation method thereof | |
| CN109400767A (en) | A kind of synthetic method being crosslinked bagasse xylan -4- acetylamino cinnamate-g-AM | |
| CN102603982A (en) | Method for preparing unsaturated carboxylic acid grafted polypropylene copolymer | |
| JP3182293B2 (en) | Water level measurement system | |
| Bevington et al. | The polymerization of acetaldehyde at low temperatures | |
| CN105572115A (en) | Method for extracting fat in non-dairy creamer and method for determining peroxidation value of non-dairy creamer | |
| CN202398144U (en) | Separating device of secondary water-cooling product of methanol pre-rectifying tower | |
| CN109187386A (en) | For detecting gel and its application of Organophosphorus and carbamate pesticides class pesticide concentration | |
| CN105510476A (en) | Method for measuring formaldehyde in textile | |
| Kuntz et al. | Copolymerization of isobutylene with 1, 4‐13C‐isoprene | |
| CN205527739U (en) | Device of preparation chlorine dioxide water treatment agent | |
| Goldfinger et al. | On the Mechanism of Inhibition of Styrene Polymerization. | |
| CA2536651A1 (en) | Microcrystalline cellulose and method for making | |
| Cristallini et al. | Kinetics and reaction mechanism of template polymerization investigated by conductimetric measurements. 2. Radical polymerization of sodium methacrylate in the presence of poly (allylamine) hydrochloride | |
| CN117309793B (en) | Method for measuring polymer of styrene device | |
| CN109030166A (en) | For detecting gel and its application of Organophosphorus and carbamate pesticides class pesticide concentration | |
| CN112250481A (en) | Kitchen waste anaerobic digestion intelligent monitoring and safety early warning system and method | |
| CN106046220B (en) | Vinyl acetate and the anti-riot poly- method of controlling security of acetic acid mixed liquor | |
| CN107921762A (en) | Multilayer film comprising propylene-ethylene-1-butene terpolymer | |
| CN112683823A (en) | Detection reagent for detecting total nitrogen content in wastewater and preparation method | |
| Doi et al. | Molecular weight distribution and stereoregularity of polypropylenes obtained with Ti (OC4H9) 4Al2 (C2H5) 3Cl3 catalyst system | |
| CN108184846A (en) | A kind of gibberellic acid missible oil and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190705 |