CN116934175A - Technical method for quality monitoring in negative resin amplification production process - Google Patents
Technical method for quality monitoring in negative resin amplification production process Download PDFInfo
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- CN116934175A CN116934175A CN202311069009.3A CN202311069009A CN116934175A CN 116934175 A CN116934175 A CN 116934175A CN 202311069009 A CN202311069009 A CN 202311069009A CN 116934175 A CN116934175 A CN 116934175A
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- 239000011347 resin Substances 0.000 title claims abstract description 94
- 229920005989 resin Polymers 0.000 title claims abstract description 94
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000012544 monitoring process Methods 0.000 title claims abstract description 18
- 230000003321 amplification Effects 0.000 title claims abstract description 11
- 238000003199 nucleic acid amplification method Methods 0.000 title claims abstract description 11
- 238000005070 sampling Methods 0.000 claims abstract description 43
- 238000004458 analytical method Methods 0.000 claims abstract description 36
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 230000002159 abnormal effect Effects 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 238000007619 statistical method Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 description 12
- 238000011020 pilot scale process Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
The invention discloses a technical method for monitoring quality of a negative resin amplification production process, which comprises the following steps: determining each key production link D1-D5 after the resin polymerization reaction and setting sampling points A1-A5 respectively; sampling analysis is carried out on the resin at sampling points A1-A5; determining key parameters of resin sampling analysis; taking key parameters of qualified resin products in a laboratory as standard data; resin parameters sampled at sampling points A1-A5 are respectively compared with standard data, and influence factors in a production link are determined; and adjusting the influencing factors, repeatedly carrying out production and sampling analysis, respectively comparing the resin parameters of the repeated sampling analysis with standard data, and locking and eliminating the influencing factors by comparing the resin parameters with the standard data. The invention adopts the technical method for monitoring the quality of the negative resin in the amplifying production process, achieves the aim of rapidly eliminating influencing factors, and achieves the stability of the product quality in the shortest time.
Description
Technical Field
The invention relates to the technical field of quality monitoring, in particular to a technical method for quality monitoring in the process of negative resin amplification production.
Background
Because PI negative resin is unstable in property, the PI negative resin is easily crosslinked under the influence of various factors in the production process, so that the quality of a final product cannot be ensured, and in order to ensure the final quality and stability of the product, the influence factors in the production process need to be eliminated and eliminated. In the process of amplifying from laboratory pilot scale to actual production pilot scale, the influence factors of all production links cause problems of the final product, so that the pilot scale process is difficult to examine, normal production cannot be realized for a long time, and the production efficiency is serious, and therefore, a quality monitoring method for rapidly eliminating the influence factors is needed.
Disclosure of Invention
The invention aims to provide a technical method for monitoring the quality of a negative resin amplification production process, which is characterized in that the resin is subjected to targeted sampling in each process link after polymerization reaction, and key technical indexes are selected for analysis and comparison, so that the aim of rapidly eliminating influence factors is fulfilled, and the stability of the product quality is realized in the shortest time.
In order to achieve the above purpose, the invention provides a technical method for monitoring the quality of a negative resin amplification production process, which comprises the following steps:
s1, determining each key production link D1-D5 after the resin polymerization reaction, and setting sampling points A1-A5 at the production links D1-D5 respectively after the polymerization reaction;
s2, carrying out sampling analysis on the resin at sampling points A1-A5;
s3, determining key parameters of resin sampling analysis;
s4, taking key parameters of qualified resin products in a laboratory as standard data;
s5, respectively comparing the resin parameters sampled at the sampling points A1-A5 with standard data, and determining influencing factors in the production link;
s6, adjusting the influencing factors, repeatedly carrying out production and sampling analysis, respectively comparing the resin parameters of the repeated sampling analysis with standard data, and locking and eliminating the influencing factors by comparing the resin parameters with the standard data.
Preferably, in step S1, production links D1-D5: d1 is polymerization reaction, D2 is impurity removal after reaction, D3 is resin molding, D4 is resin refining, and D5 is processed into a resin finished product;
the samples at sampling points A1-A5 were: a1 reaction liquid, A2 reaction liquid after impurity removal, A3 molding resin, A4 refined resin and A5 resin products.
Preferably, the sampling analysis in step S2 is to analyze the viscosity and molecular weight of the sample, and the analysis method includes:
s21, determining a viscosity value by applying shearing force and measuring reaction of the sample fluid by using a cone-plate viscometer;
s22, measuring the molecular weight of the sample by a gas gel chromatograph, and detecting the weight average molecular weight and the number average molecular weight and the dispersity.
Preferably, the step S3 specifically includes the following steps:
s31, setting a normal deviation range by taking the analysis viscosity and the molecular weight of the standard resin as reference values, and taking the normal deviation range as a standard value of analysis comparison, if the viscosity value and the molecular weight of a sample are within the range, the quality of the resin is qualified, and if the viscosity value and the molecular weight of the sample are not within the range, the quality of the resin is not qualified;
s32, comparing the viscosity and the molecular weight of the resin with qualified quality and the resin with unqualified quality, and taking unqualified parameters as key parameters.
Preferably, step S4 is to take 5 qualified batches of resin in the laboratory, divide each batch of resin into 5 samples, analyze each sample to obtain 25 sets of data, select 50% of solid content viscosity data for statistical analysis, and determine the reference standard data and deviation range.
Preferably, in step S5, if the analysis parameter of the sampling point resin is within the deviation range of the standard data, it indicates that the production link is normal, and if the analysis parameter of the sampling point resin is not within the deviation range of the standard data, it indicates that the production link has an abnormal influence factor.
Preferably, the number of repetitions in step S6 is 3.
The invention has the following advantages:
according to the invention, the resin is subjected to targeted sampling in each process link after polymerization reaction, and key technical indexes are selected for analysis and comparison, so that the purpose of rapidly eliminating influence factors is realized, and the stability of product quality is realized in the shortest time.
The invention can rapidly determine that if a plurality of influencing factors exist in the production links with problems, the production links can be examined in sections by utilizing a plurality of times, and one production link can be examined each time.
The invention solves the problems that the prior production process is influenced by multiple factors, and the pilot scale production with stable product quality can not be realized for a long time.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a flow chart of a technical method for quality monitoring in a negative resin amplification production process of the present invention;
FIG. 2 is a schematic diagram of the relationship between the production links and the sampling points according to the present invention.
Detailed Description
The invention will be further described with reference to examples. Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The above-mentioned features of the invention or the features mentioned in the specific examples can be combined in any desired manner, and these specific examples are only intended to illustrate the invention and are not intended to limit the scope of the invention.
Examples
Referring to fig. 1 to 2, as shown in the drawings, a technical method for quality monitoring in a negative resin amplification production process includes the following steps: s1, determining each key production link D1-D5 after resin polymerization, wherein D1 is polymerization, D2 is impurity removal after reaction, D3 is resin molding, D4 is resin refining, and D5 is processed into a resin finished product. Sampling points A1 to A5 are respectively set in production links D1 to D5 after the polymerization reaction, and samples at the sampling points A1 to A5 are respectively: a1 reaction liquid, A2 reaction liquid after impurity removal, A3 molding resin, A4 refined resin and A5 resin products.
S2, carrying out sampling analysis on the resin at sampling points A1-A5, and analyzing the viscosity and molecular weight of the sample, wherein the analysis method comprises the following steps:
s21, determining a viscosity value by applying shearing force and measuring reaction of the sample fluid by using a cone-plate viscometer;
s22, measuring the molecular weight of the sample by a gas gel chromatograph, and detecting the weight average molecular weight and the number average molecular weight and the dispersity.
S3, determining key parameters of resin sampling analysis;
s31, setting a normal deviation range by taking the analysis viscosity and the molecular weight of the standard resin as reference values, and taking the normal deviation range as a standard value of analysis comparison, if the viscosity value and the molecular weight of a sample are within the range, the quality of the resin is qualified, and if the viscosity value and the molecular weight of the sample are not within the range, the quality of the resin is not qualified;
s32, comparing the viscosity and the molecular weight of the resin with qualified quality and the resin with unqualified quality, and taking unqualified parameters as key parameters.
S4, taking key parameters of qualified resin products in a laboratory as standard data;
taking 5 qualified batches of resin in a laboratory, dividing each batch of resin into 5 samples, analyzing each sample to obtain 25 groups of data, selecting 50% solid content viscosity data for statistical analysis, and determining reference standard data and deviation range.
Average value of solids content viscosity= (solids content viscosity data 1+data 2+.+ data n)/n;
standard deviation of solids viscosity = sqrt (((solids viscosity data 1-average)/(2+ (solids viscosity data 2-average)/(2+) + (solids viscosity data n-average)/(2)/n);
solid content viscosity deviation range: solid content viscosity average ± standard deviation.
S5, respectively comparing the resin parameters sampled at the sampling points A1-A5 with standard data, and determining influencing factors in the production link;
if the analysis parameters of the sampling point resin are within the deviation range of the standard data, the normal production link is indicated, and if the analysis parameters of the sampling point resin are not within the deviation range of the standard data, the abnormal influence factors exist in the production link.
S6, adjusting the influencing factors, repeatedly carrying out production and sampling analysis, respectively comparing the resin parameters of the repeated sampling analysis with standard data, and locking and eliminating the influencing factors by comparing the resin parameters with the standard data. The repeated times are 3 times, so that the verification accuracy is ensured.
Therefore, the invention adopts the technical method for monitoring the quality of the negative resin amplification production process, the resin is subjected to targeted sampling in each process link after the polymerization reaction, and key technical indexes are selected for analysis and comparison, so that the aim of rapidly eliminating influence factors is fulfilled, and the stability of the product quality is realized in the shortest time. If a plurality of influencing factors exist in the production links with problems, the production links with problems can be rapidly determined, and the sectional investigation can be performed by utilizing the production for a plurality of times, and one production link can be inspected each time. Solves the problems that the prior production process is influenced by multiple factors and the pilot scale production with stable product quality can not be realized for a long time.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (7)
1. The technical method for monitoring the quality of the negative resin amplification production process is characterized by comprising the following steps of:
s1, determining each key production link D1-D5 after the resin polymerization reaction, and setting sampling points A1-A5 at the production links D1-D5 respectively after the polymerization reaction;
s2, carrying out sampling analysis on the resin at sampling points A1-A5;
s3, determining key parameters of resin sampling analysis;
s4, taking key parameters of qualified resin products in a laboratory as standard data;
s5, respectively comparing the resin parameters sampled at the sampling points A1-A5 with standard data, and determining influencing factors in the production link;
s6, adjusting the influencing factors, repeatedly carrying out production and sampling analysis, respectively comparing the resin parameters of the repeated sampling analysis with standard data, and locking and eliminating the influencing factors by comparing the resin parameters with the standard data.
2. The method for monitoring the quality of a negative resin amplification production process according to claim 1, wherein the production steps D1 to D5 in step S1 are as follows: d1 is polymerization reaction, D2 is impurity removal after reaction, D3 is resin molding, D4 is resin refining, and D5 is processed into a resin finished product;
the samples at sampling points A1-A5 were: a1 reaction liquid, A2 reaction liquid after impurity removal, A3 molding resin, A4 refined resin and A5 resin products.
3. The method according to claim 1, wherein the step S2 of sampling analysis is to analyze the viscosity and molecular weight of the sample, and the analysis method comprises:
s21, determining a viscosity value by applying shearing force and measuring reaction of the sample fluid by using a cone-plate viscometer;
s22, measuring the molecular weight of the sample by a gas gel chromatograph, and detecting the weight average molecular weight and the number average molecular weight and the dispersity.
4. The method for monitoring the quality of the production process of amplifying negative resin according to claim 1, wherein the step S3 specifically comprises the following steps:
s31, setting a normal deviation range by taking the analysis viscosity and the molecular weight of the standard resin as reference values, and taking the normal deviation range as a standard value of analysis comparison, if the viscosity value and the molecular weight of a sample are within the range, the quality of the resin is qualified, and if the viscosity value and the molecular weight of the sample are not within the range, the quality of the resin is not qualified;
s32, comparing the viscosity and the molecular weight of the resin with qualified quality and the resin with unqualified quality, and taking unqualified parameters as key parameters.
5. The technical method for monitoring the quality of the production process of amplifying the negative resin according to claim 1, which is characterized in that: and S4, taking 5 qualified batches of resin in a laboratory, dividing each batch of resin into 5 samples, analyzing each sample to obtain 25 groups of data, selecting 50% solid content viscosity data for statistical analysis, and determining reference standard data and deviation ranges.
6. The technical method for monitoring the quality of the production process of amplifying the negative resin according to claim 1, which is characterized in that: in step S5, if the analysis parameter of the sampling point resin is within the deviation range of the standard data, the production link is normal, and if the analysis parameter of the sampling point resin is not within the deviation range of the standard data, the production link has an abnormal influence factor.
7. The technical method for monitoring the quality of the production process of amplifying the negative resin according to claim 1, which is characterized in that: the number of repetitions in step S6 is 3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117522100A (en) * | 2023-11-16 | 2024-02-06 | 永久电力金具有限公司 | Optimization method for electric power fitting production process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117522100A (en) * | 2023-11-16 | 2024-02-06 | 永久电力金具有限公司 | Optimization method for electric power fitting production process |
| CN117522100B (en) * | 2023-11-16 | 2024-04-05 | 永久电力金具有限公司 | Optimization method for electric power fitting production process |
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