CN115235951A - Method for online viscosity detection of nylon 6 production process - Google Patents
Method for online viscosity detection of nylon 6 production process Download PDFInfo
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- CN115235951A CN115235951A CN202210876744.4A CN202210876744A CN115235951A CN 115235951 A CN115235951 A CN 115235951A CN 202210876744 A CN202210876744 A CN 202210876744A CN 115235951 A CN115235951 A CN 115235951A
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- nylon
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 14
- 238000001514 detection method Methods 0.000 title claims description 22
- 239000000523 sample Substances 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000013499 data model Methods 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000010183 spectrum analysis Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- 230000008859 change Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000005070 sampling Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N2011/006—Determining flow properties indirectly by measuring other parameters of the system
- G01N2011/008—Determining flow properties indirectly by measuring other parameters of the system optical properties
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The utility model provides a method for nylon 6 production technology on-line viscosity detects, can make wet section be detected by infrared viscometer through setting up the riffle, sets up the riffle respectively at the left and right sides of shale shaker, through setting up two riffles, disposes two infrared viscometer, can play multidata contrast, ensures the accuracy nature of wet section viscosity data.
Description
Technical Field
The invention relates to the technical field of nylon 6 production detection, in particular to a method for detecting the on-line viscosity of a nylon 6 production process.
Background
In the industrial production of nylon 6, caprolactam, a ring-opening agent and a chain terminating agent are used for polymerization reaction to generate a melt, a granulator is used for cutting into slices under the action of water cooling, and then impurity extraction, moisture drying and solid phase tackifying are carried out to generate dry slices. The pellets produced by the pelletizer are referred to as wet pellets. When the production process fluctuates, in order to produce high-quality slices, the viscosity of the wet slices is often required to be detected so as to find out the change of the viscosity index in the process in time, and the viscosity index of the wet slices is adjusted in the solid-phase tackifying process so as to achieve the purpose of stabilizing the product index.
The inventor finds that in the actual production process, the conventional laboratory detection method is a sulfuric acid method, wet slices need to be dried, dissolved in concentrated sulfuric acid under the condition of heating and stirring, and then the outflow time of the sulfuric acid solution of the slices is measured by an Ubbelohde viscometer and compared with the outflow time of the concentrated sulfuric acid, so as to obtain the viscosity of the wet slices. The detection method has a long period, and after the wet slice viscosity data is obtained, the process adjustment of solid-phase tackifying is carried out according to the wet slice viscosity, so that the hysteresis is always caused, the adjustment is not timely, and the high quality rate of the product is influenced.
Disclosure of Invention
In order to overcome the defects of the technology, the invention provides a method for online viscosity detection of a nylon 6 production process, which can provide the viscosity indication change of a wet section in real time and provide timeliness for the process adjustment of subsequent system solid-phase tackifying.
The technical scheme adopted by the invention for overcoming the technical problems is as follows:
a method for detecting the on-line viscosity of a nylon 6 production process is characterized by comprising the following steps:
a) Connecting a feed inlet of a granulator with a discharge outlet of a polymerization system, and enabling the granulator to produce wet slices;
b) Communicating a feed inlet of a drying machine with a discharge outlet of a granulator, feeding wet slices and water generated by the granulator into the drying machine, and carrying out slicing and water separation by the drying machine;
c) Communicating a feed port of a vibrating screen with a discharge port of a spin dryer, arranging sample separators at the left end and the right end of the vibrating screen, and enabling wet slices to enter the sample separators under the flow guidance of the vibrating screen;
d) And an infrared viscometer is arranged on one side of the sample splitter, an infrared probe of the infrared viscometer irradiates infrared rays on the wet slices in the sample splitter, and the viscosity values of the wet slices are obtained after spectral analysis and data model calculation.
Furthermore, above-mentioned riffle sampler is the U font structure, has the guiding gutter in the riffle sampler, the lower terminal surface of guiding gutter is parallel and level mutually with the up end of shale shaker screen cloth.
Furthermore, the sample divider is fixed at the side end of the vibrating screen through a bolt.
Furthermore, still include the current-limiting plate that sets up in the both ends about the riffle sampler along vertical direction respectively, the current-limiting plate inserts in the guiding gutter, and the last postpone width direction of current-limiting plate is provided with N opening.
Preferably, N is 3.
The invention has the beneficial effects that:
1. can make wet section by infrared viscometer detection through setting up the riffle sampler, set up the riffle sampler respectively at the left and right sides both ends of shale shaker, through setting up two riffle samplers, dispose two infrared viscometer, can play multidata contrast, ensure the accuracy nature of wet section viscosity data.
2. Compared with a laboratory sulfuric acid method, the on-line viscometer designed by the invention has simpler operation and higher efficiency.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic top view of the shaker section of the present invention;
FIG. 3 is a side view schematic of a shaker section of the present invention;
FIG. 4 is a schematic structural view of a restrictor plate of the present invention;
in the figure, 1 is a sample divider 2, a flow limiting plate 3, a feed inlet 4, a discharge outlet 5, a wet slice 6 and an infrared viscometer.
Detailed Description
The present invention is further described with reference to fig. 1 to 4.
Example 1:
a method for detecting the on-line viscosity of a nylon 6 production process is characterized by comprising the following steps:
a) The feed port of the pelletizer, which produces wet chips 5, was connected to the discharge port of the polymerization system.
b) And a feed inlet of the drying machine is communicated with a discharge outlet of the granulator, wet slices 5 and water generated by the granulator enter the drying machine, and the drying machine performs slicing and water separation.
c) A feed inlet 3 of the vibrating screen is communicated with a discharge outlet of the spin dryer, sample distributors 1 are arranged at the left end and the right end of the vibrating screen, and wet slices 5 enter the sample distributors 1 under the flow guidance of the vibrating screen.
d) An infrared viscometer 6 is arranged on one side of the sample splitter 1, an infrared probe of the infrared viscometer 6 irradiates infrared rays on the wet slice 5 in the sample splitter, and the viscosity value of the wet slice 5 is obtained after spectral analysis and data model calculation. The infrared viscometer 6 comprises a main light source, an optical acquisition calibration module and a spectrometer, a detection port of the infrared viscometer vertically irradiates a slice layer in the sample splitter, and the viscosity is measured by utilizing the difference of the absorption degree of infrared rays by the chemical bonds of wet slices 5 of different years and the difference of the intensity of the reflected infrared rays. In the early stage, a data model of different years and infrared ray absorptivities is established by using conventional viscosity detection data provided by a chemical chamber.
Can make wet section 5 detected by infrared viscometer 6 through setting up riffle 1, set up riffle 1 respectively at the left and right sides both ends of shale shaker, through setting up two rifflers 1, dispose two infrared viscometers 6, can play multidata contrast, ensure the accuracy nature of 5 viscosity data in wet section.
The sample divider is of a U-shaped structure, a flow guide groove is formed in the sample divider, and the lower end face of the flow guide groove is flush with the upper end face of the vibrating screen. Therefore, under the action of the vibrating screen, the wet slice 5 moves backwards, enters the diversion trench of the sample divider and moves in the diversion trench.
Preferably, the sample splitter is fixed to the side end of the vibrating screen by bolts. The sample splitter is installed through the bolts, and is simple in structure and convenient to install and disassemble.
Furthermore, still including setting up the current-limiting plate 2 in the both ends about the riffle sampler 1 along vertical direction respectively, current-limiting plate 2 inserts in the guiding gutter, and the last delay width direction of current-limiting plate 2 is provided with N opening. The preferred value of N is 3. The wet slices 5 in the sample splitter can only flow forwards through the opening, so that the slice flow layer at the detection point part of the infrared viscometer 6 is uniform under the action of the restrictor plate 2, and the thickness and the flow rate of the wet slices 5 are kept consistent so as to reduce errors.
Example 2:
under the continuous production working condition, the invention can provide the real-time and continuous viscosity value and viscosity change trend of the wet slice 5 after being applied, so that an operator can monitor the viscosity change conveniently; if the viscosity change deviates from the high-grade product index, an operator can adjust the production index in time to stabilize the viscosity and improve the high-grade product rate.
Example 3:
under the continuous production working condition, the method can remove the links of sampling, reagent configuration, wet slice viscosity detection and the like after being applied, and realizes the full-automatic detection of the wet slice viscosity.
Comparative example 1:
for sample detection under the working condition of the embodiment 2, the viscosity of wet slices detected in a laboratory needs to be measured by sampling, drying, dissolving in concentrated sulfuric acid under the condition of heating and stirring, measuring the outflow time of a slice sulfuric acid solution by using a black-type viscometer and comparing with the outflow time of the concentrated sulfuric acid to obtain the viscosity of the wet slices, wherein the total time is about 6 hours; compared with a viscosity detection method for wet slices in a laboratory, the method has the advantages of instantaneity, timeliness and continuity.
Comparative example 2:
for sample detection under the working condition of embodiment 3, one operator is required for sampling in laboratory detection of wet slice viscosity, one laboratory worker is provided with an experimental reagent, and one laboratory worker is used for analysis and detection. Compared with a method for detecting the viscosity of the wet slice in a laboratory, the method has the advantages that the medicine configuration is removed, and the cost is saved; personnel sampling and personnel analysis and detection are removed, frequent operation of people is reduced, and the advantages of unmanned and automatic production are achieved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for detecting the on-line viscosity of a nylon 6 production process is characterized by comprising the following steps:
a) Connecting a feed inlet of a granulator with a discharge outlet of a polymerization system, wherein the granulator generates wet slices (5);
b) A feed inlet of the drying machine is communicated with a discharge outlet of the granulator, wet slices (5) and water generated by the granulator enter the drying machine, and the drying machine carries out slicing and water separation;
c) A feed inlet (3) of a vibrating screen is communicated with a discharge outlet of a spin dryer, sample distributors (1) are arranged at the left end and the right end of the vibrating screen, and wet slices (5) enter the sample distributors (1) under the flow guidance of the vibrating screen;
d) An infrared viscometer (6) is arranged on one side of the sample splitter (1), an infrared probe of the infrared viscometer (6) irradiates infrared rays on the wet section (5) in the sample splitter, and the viscosity value of the wet section (5) is obtained after spectral analysis and data model calculation.
2. The method for on-line viscosity detection of nylon 6 production process according to claim 1, characterized in that: the riffle sampler is U font structure, has the guiding gutter in the riffle sampler, the lower terminal surface of guiding gutter is parallel and level mutually with the up end of shale shaker screen cloth.
3. The method for on-line viscosity detection of nylon 6 production process of claim 1, characterized by: the sample splitter is fixed at the side end of the vibrating screen through bolts.
4. The method for on-line viscosity detection of nylon 6 production process of claim 2, characterized by: the sample splitter is characterized by further comprising flow limiting plates (2) which are arranged at the left end and the right end of the sample splitter (1) in the vertical direction respectively, the flow limiting plates (2) are inserted into the flow guide grooves, and N openings are formed in the flow limiting plates (2) in the delay width direction.
5. The method for on-line viscosity detection of nylon 6 production process according to claim 4, characterized in that: the value of N is 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210876744.4A CN115235951A (en) | 2022-07-25 | 2022-07-25 | Method for online viscosity detection of nylon 6 production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210876744.4A CN115235951A (en) | 2022-07-25 | 2022-07-25 | Method for online viscosity detection of nylon 6 production process |
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| CN115235951A true CN115235951A (en) | 2022-10-25 |
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| CN202210876744.4A Pending CN115235951A (en) | 2022-07-25 | 2022-07-25 | Method for online viscosity detection of nylon 6 production process |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107703099A (en) * | 2016-08-08 | 2018-02-16 | 中国石油化工股份有限公司 | On-line continuous detection device and method and polymerization reaction system and method |
| CN112094406A (en) * | 2020-08-31 | 2020-12-18 | 聊城鲁西聚酰胺新材料科技有限公司 | Nylon 6 production process and system and product thereof |
| CN114505978A (en) * | 2022-03-11 | 2022-05-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Online index detection device, production system and method for nylon 6 dry slices |
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2022
- 2022-07-25 CN CN202210876744.4A patent/CN115235951A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107703099A (en) * | 2016-08-08 | 2018-02-16 | 中国石油化工股份有限公司 | On-line continuous detection device and method and polymerization reaction system and method |
| CN112094406A (en) * | 2020-08-31 | 2020-12-18 | 聊城鲁西聚酰胺新材料科技有限公司 | Nylon 6 production process and system and product thereof |
| CN114505978A (en) * | 2022-03-11 | 2022-05-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Online index detection device, production system and method for nylon 6 dry slices |
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