A method for preparing organic pigment suitable for PP spinning

By adopting methods suitable for PP wire extraction in organic pigment production, customer matching inspection methods are established, diazotization reaction and real-time temperature observation are carried out, the problem of pigment hue and coloring force deviation is solved, and the efficiency of pigment, economical production and supply chain stability are achieved.

CN114659991BActive Publication Date: 2025-03-14CROWN CHEMICAL CORP
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Patent Information

Application Number
CN202210293289.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-03-24
Publication Date
2025-03-14
Estimated Expiration
2042-03-24

AI Technical Summary

Technical Problem

In the existing organic pigment production technology, there are deviations in the hue and chromatic power of the detected pigment, and customers lack effective information feedback when judging the color of the pigment, resulting in disconnection of the supply chain.

Method used

The organic pigment production method suitable for PP wire extraction is adopted, including establishing a pigment inspection method that matches customers, adjusting the pigment production process through diazotization reaction, and conducting real-time temperature observation to ensure that the pigment hue and coloring power meet the standards.

Benefits of technology

Through injection molding and tableting processes, the color of the PP color sheet is similar to that of the PP fiber, which solves the color judgment problem; the amount of rosin used meets the balance of dispersion and hiding power, and the addition of strontium chloride and calcium chloride improves the heat resistance and coloring power of the pigment, reducing production costs.

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Abstract

The invention relates to the technical field of organic pigment production, and in particular to a method for producing an organic pigment suitable for PP spinning. In view of the fact that the existing organic pigment production technology has deviations in the pigment hue and tinting power detected by the inspection method used in the production process, and no effective information is fed back to the pigment production process when the customer judges the color of the pigment, resulting in a disconnection in the supply chain, the following scheme is proposed, which includes the following steps: S1: method establishment, S2: sampling measurement, S3: pigment adjustment, S4: real-time observation. The purpose of the invention is to make the pigment color presented by the prepared PP color sheet similar to the color presented by the PP fiber by means of injection molding first and then tableting, thereby solving the color judgment problem. At the same time, the amount of rosin used just meets the balance requirements of dispersibility and hiding power, and the addition of strontium chloride and calcium chloride improves the heat resistance and tinting power of the pigment, thereby reducing the production cost of the pigment.
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Description

Technical Field

[0001] The invention relates to the technical field of organic pigment production, and in particular to a method for producing an organic pigment suitable for PP spinning. Background Art

[0002] As a dye, organic pigments have the advantages of bright colors, strong tinting power, and non-toxicity. However, some of their varieties are not as good as inorganic pigments in terms of light resistance, heat resistance, solvent resistance, and migration resistance. With the development of organic pigment technology, its shortcomings have been improved and its application areas have been further expanded. At present, organic pigments are widely used in inks, paints, coatings, synthetic fiber pulp coloring, plastic and rubber coloring, etc. With the increasing market demand for high-end organic pigments, my country's organic pigment manufacturers are paying more and more attention to the development of high-performance pigments, and the industry will gradually develop towards high-end.

[0003] However, the existing organic pigment production technology has the problem that the pigment hue and tinting strength detected by the inspection method used in the production process are deviated, and there is no effective information feedback to the pigment production process when customers judge the color of the pigment, resulting in a disconnection in the supply chain. Therefore, we propose an organic pigment production method suitable for PP spinning to solve the above problems. Summary of the invention

[0004] The purpose of the present invention is to solve the problems in the current organic pigment production technology, such as the deviation of pigment hue and tinting strength detected by the inspection method adopted in the production process, and the lack of effective information feedback to the pigment production process when customers judge the color of the pigment, resulting in a disconnection in the supply chain. A method for producing organic pigments suitable for PP spinning is proposed.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A method for preparing an organic pigment suitable for PP spinning, comprising the following steps:

[0007] S1: Method establishment: Professionals establish pigment inspection methods that match customers;

[0008] S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, and processing is performed based on the measurement results;

[0009] S3: Adjusting pigments: Adjusting the pigment production process through diazotization reaction and observing the reaction temperature of the reaction process in real time;

[0010] S4: Real-time observation: During the diazotization reaction, the reaction temperature is manually observed in real time through a temperature detector, and processing is performed based on the observed results;

[0011] S5: Customer inspection: Produce the obtained ratio according to the test and send samples to the customer for inspection. The inspection determines whether the finished product samples are qualified;

[0012] Preferably, in S1, professionals establish a pigment inspection method that matches the customer, by using the inspection material polypropylene (PP) that is consistent with the customer, without using a spinning machine, and using an injection molding machine and a vulcanizer for inspection and color matching. When inspecting and matching, the pigment is first dispersed in polypropylene (PP) at 220-300°C using an injection molding machine to make a color plate, and the color plate of the standard sample and the sample prepared in the same period are placed side by side in a vulcanizer to be pressed into a 0.5-0.6mm thin sheet. After the pressing is completed, the pressed thin sheet is subjected to color difference comparison under bright light, and pigments matching the hiding power, hue and tinting power are selected for adjustment, so that the color difference between the sample and the standard is gradually reduced, and the transparent color and the surface color need to be considered at the same time to balance the two. The sample obtained in this way is composed of multiple batches of pigments in a certain proportion, not only the strong color, but also the diluted color in the same proportion as the strong color, which is also made into a 0.5-0.6mm thin sheet, and the sample is compared with the standard, and the tinting power difference is adjusted to be less than or equal to 2% by comparison;

[0013] Preferably, in S2, the thin slices formed after pressing are sampled and measured, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin slices in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and after the technician arrives The thin film measurement data is fed back manually, and the technician debugs the vulcanizer based on the fedback data. A pressing test is required for each debugging. The thickness of the thin film obtained by the pressing test is measured manually, and the process is performed based on the thickness measurement result. If the measurement result shows that the thin film thickness data obtained by the pressing test is within the required data range, the vulcanizer is not shut down, and the thin film pressing step is performed. If the measurement result shows that the thin film thickness data obtained by the pressing test is not within the required data range, the vulcanizer is shut down, and the technician continues to debug until the thin film thickness data obtained by the pressing test after debugging is within the required data range, and the debugging is stopped;

[0014] Preferably, in S3, the pigment production process is adjusted by diazotization reaction, and the pigment presents a hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as a diazo component, and the raw material is formed into fine particles by dissolving and acid precipitation, and the reaction temperature is controlled at 5-15°C under acidic conditions for diazotization reaction, wherein during the diazotization reaction, after adding sodium nitrite solution, starch potassium iodide test paper is used for detection until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is performed, and the reaction is continued for 1 hour, and the starch iodide is kept The potassium chloride test paper has color, and the process uses 2,3 acid as a coupling component, and the dissolved 2,3 acid is coupled with a diazo solution, and the coupling process needs to control the pH value during coupling, and the pH value at the coupling end point is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the end point pH value, and the addition ratio of rosin is 2-3%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:1;

[0015] Preferably, in S4, when the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is judged, and the judgment result is processed, wherein the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction, and the reaction is continued if it is judged to be a normal reaction, and vaporized pure water is blown into the reaction device through a blower if it is judged to be an abnormal reaction, wherein the temperature of the vaporized pure water is maintained at 1-5°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed, wherein if the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed, and if the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the blowing amount per unit time of the vaporized pure water is manually increased;

[0016] Preferably, in S5, the obtained ratio is produced according to the test and samples are sent to customers for inspection, wherein the inspection is carried out by mixing and crushing different batches of dry pigments in the ratio table according to this ratio, and the final product is tested, wherein the finished product inspection is carried out according to the above-mentioned inspection method, and after the inspection is completed, 100g of finished product samples are sent to the customer for confirmation, and the customer draws the pigment into PP fiber, compares it with PP fiber made of standard pigment, and judges whether the finished product sample is qualified through comparison result, and the customer provides feedback on the judgment result.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] 1. By injection molding first and then tableting, the pigment color of the prepared PP color sheet is similar to the color of the PP fiber, solving the color judgment problem.

[0019] 2. The amount of rosin used just meets the balance requirements of dispersibility and hiding power, and the addition of strontium chloride and calcium chloride improves the heat resistance and tinting power of the pigment, reducing the production cost of the pigment.

[0020] The purpose of the present invention is to make the color of the pigment presented by the prepared PP color sheet similar to the color presented by the PP fiber by means of injection molding first and then tableting, thereby solving the color judgment problem. At the same time, the amount of rosin used just meets the balance requirements of dispersibility and hiding power, and the addition of strontium chloride and calcium chloride improves the heat resistance and tinting power of the pigment, thereby reducing the production cost of the pigment. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The present invention provides a flow chart of a method for producing an organic pigment suitable for PP spinning. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Example 1

[0023] Reference Figure 1 A method for preparing an organic pigment suitable for PP spinning comprises the following steps:

[0024] S1: Method establishment: Professionals establish a pigment inspection method that matches the customer. By using the inspection material polypropylene (PP) that is consistent with the customer, and not using a spinning machine, and using an injection molding machine and a vulcanizer for inspection and color matching, the pigment is first dispersed in polypropylene (PP) at 270°C using an injection molding machine to make a color plate, and the color plates of the standard sample and the test sample prepared at the same time are placed side by side in a vulcanizer to be pressed into a 0.55mm thin sheet. After the pressing is completed, the pressed thin sheet is compared under bright light for color difference, and pigments that match the hiding power, hue and tinting power are selected for adjustment, so that the color difference between the sample and the standard is gradually reduced. At the same time, the transparent color and the surface color need to be considered at the same time to balance the two. The sample obtained in this way is composed of multiple batches of pigments in a certain proportion, not only the strong color, but also the diluted color with the same proportion as the strong color, which is also made into a 0.55mm thin sheet, and the sample is compared with the standard. By comparison, the tinting power difference is adjusted to be less than or equal to 2%;

[0025] S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin sheets in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and the technician arrives and is Manually perform sheet measurement data feedback, and the technician debugs the vulcanizer based on the feedback data. A pressing test is required for each debugging, and the thickness of the sheet obtained by the pressing test is manually measured, and the thickness measurement result is processed. If the measurement result shows that the sheet thickness data obtained by the pressing test is within the required data range, the vulcanizer is not shut down, and the sheet pressing step is performed. If the measurement result shows that the sheet thickness data obtained by the pressing test is not within the required data range, the vulcanizer is shut down, and the technician continues to debug until the sheet thickness data obtained by the pressing test after debugging is within the required data range, and then the debugging is stopped;

[0026] S3: Adjusting the pigment: Adjusting the pigment production process through diazotization reaction, making the pigment present the hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as the diazo component, and the raw material is formed into fine particles by dissolving and acid precipitation, and the reaction temperature is controlled at 5-15°C under acidic conditions for diazotization reaction, wherein during the diazotization reaction, after adding sodium nitrite solution, starch potassium iodide test paper is used for detection until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is carried out, and the reaction is continued for 1 hour to keep the starch iodide solution. The potassium test paper has color, and the process uses 2,3 acid as a coupling component, and the dissolved 2,3 acid is coupled with a diazo solution, and the coupling process needs to control the pH value during coupling, and the pH value at the coupling end point is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the end point pH value, and the addition ratio of rosin is 2.5%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:1;

[0027] S4: Real-time observation: When the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is judged, and the judgment result is processed. If the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and if the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction. If it is judged to be a normal reaction, the reaction is continued. If it is judged to be an abnormal reaction, vaporized pure water is blown into the reaction device through a blower, wherein the temperature of the vaporized pure water is maintained at 3°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the amount of vaporized pure water blown in per unit time is manually increased;

[0028] S5: Customer inspection: The obtained ratio is produced according to the test and samples are sent to customers for inspection. During the inspection, different batches of dry pigments in the ratio table are mixed and crushed according to this ratio, and the final product is tested. The finished product inspection is carried out according to the above inspection method. After the inspection is completed, 100g of finished product samples are sent to the customer for confirmation. The customer will draw the pigment into PP fiber, compare it with the PP fiber made of standard pigment, and judge whether the finished product sample is qualified based on the comparison result. At the same time, the customer will feedback the judgment result. Example 2

[0029] Reference Figure 1 A method for preparing an organic pigment suitable for PP spinning comprises the following steps:

[0030] S1: Method establishment: Professionals establish a pigment inspection method that matches the customer. By using the inspection material polypropylene (PP) that is consistent with the customer, and not using a spinning machine, and using an injection molding machine and a vulcanizer for inspection and color matching, the pigment is first dispersed in polypropylene (PP) at 220°C using an injection molding machine to make a color plate, and the color plates of the standard sample and the test sample prepared at the same time are placed side by side in a vulcanizer to be pressed into a 0.5mm thin sheet. After the pressing is completed, the pressed thin sheet is placed under bright light for color difference comparison, and pigments that match the hiding power, hue and tinting power are selected for adjustment, so that the color difference between the sample and the standard is gradually reduced. At the same time, the transparent color and the surface color need to be considered at the same time to balance the two. The sample obtained in this way is composed of multiple batches of pigments in a certain proportion, not only the strong color, but also the diluted color with the same proportion as the strong color, which is also made into a 0.5mm thin sheet, and the sample is compared with the standard. Through comparison, the tinting power difference is adjusted to be less than or equal to 2%;

[0031] S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin sheets in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and the technician arrives and is Manually perform sheet measurement data feedback, and the technician debugs the vulcanizer based on the feedback data. A pressing test is required for each debugging, and the thickness of the sheet obtained by the pressing test is manually measured, and the thickness measurement result is processed. If the measurement result shows that the sheet thickness data obtained by the pressing test is within the required data range, the vulcanizer is not shut down, and the sheet pressing step is performed. If the measurement result shows that the sheet thickness data obtained by the pressing test is not within the required data range, the vulcanizer is shut down, and the technician continues to debug until the sheet thickness data obtained by the pressing test after debugging is within the required data range, and then the debugging is stopped;

[0032] S3: Adjusting the pigment: Adjusting the pigment production process through diazotization reaction, making the pigment present the hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as the diazo component, and the raw material is formed into fine particles by dissolving and acid precipitation, and the reaction temperature is controlled at 5-15°C under acidic conditions for diazotization reaction, wherein during the diazotization reaction, sodium nitrite solution is added and then starch potassium iodide test paper is used for detection, until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is carried out, and the reaction is continued for 1 hour, and the starch iodide is kept The potassium chloride test paper has color, and the process uses 2,3 acid as a coupling component, and the dissolved 2,3 acid is coupled with a diazo solution, and the coupling process needs to control the pH value during coupling, and the pH value at the coupling end point is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the end point pH value, and the addition ratio of rosin is 2%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:1;

[0033] S4: Real-time observation: When the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is judged, and the judgment result is processed. If the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and if the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction. If it is judged to be a normal reaction, the reaction is continued. If it is judged to be an abnormal reaction, vaporized pure water is blown into the reaction device through a blower, wherein the temperature of the vaporized pure water is maintained at 1°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the amount of vaporized pure water blown in per unit time is manually increased;

[0034] S5: Customer inspection: The obtained ratio is produced according to the test and samples are sent to customers for inspection. During the inspection, different batches of dry pigments in the ratio table are mixed and crushed according to this ratio, and the final product is tested. The finished product inspection is carried out according to the above inspection method. After the inspection is completed, 100g of finished product samples are sent to the customer for confirmation. The customer will draw the pigment into PP fiber, compare it with the PP fiber made of standard pigment, and judge whether the finished product sample is qualified based on the comparison result. At the same time, the customer will feedback the judgment result. Example 3

[0035] Reference Figure 1 A method for preparing an organic pigment suitable for PP spinning comprises the following steps:

[0036] S1: Method establishment: Professionals establish a pigment inspection method that matches the customer. By using the inspection material polypropylene (PP) that is consistent with the customer, and not using a spinning machine, and using an injection molding machine and a vulcanizer for inspection and color matching, the pigment is first dispersed in polypropylene (PP) at 300°C using an injection molding machine to make a color plate, and the color plates of the standard sample and the test sample prepared at the same time are placed side by side in a vulcanizer to be pressed into a 0.6mm thin sheet. After the pressing is completed, the pressed thin sheet is compared under bright light for color difference, and pigments that match the hiding power, hue and tinting power are selected for adjustment, so that the color difference between the sample and the standard is gradually reduced. At the same time, the transparent color and the surface color need to be considered at the same time to balance the two. The sample obtained in this way is composed of multiple batches of pigments in a certain proportion, not only the strong color, but also the diluted color with the same proportion as the strong color, which is also made into a 0.6mm thin sheet, and the sample is compared with the standard. Through comparison, the tinting power difference is adjusted to be less than or equal to 2%;

[0037] S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin sheets in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and the technician arrives and is Manually perform sheet measurement data feedback, and the technician debugs the vulcanizer based on the feedback data. A pressing test is required for each debugging, and the thickness of the sheet obtained by the pressing test is manually measured, and the thickness measurement result is processed. If the measurement result shows that the sheet thickness data obtained by the pressing test is within the required data range, the vulcanizer is not shut down, and the sheet pressing step is performed. If the measurement result shows that the sheet thickness data obtained by the pressing test is not within the required data range, the vulcanizer is shut down, and the technician continues to debug until the sheet thickness data obtained by the pressing test after debugging is within the required data range, and then the debugging is stopped;

[0038] S3: Adjusting the pigment: Adjusting the pigment production process through diazotization reaction, making the pigment present the hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as the diazo component, and the raw material is formed into fine particles by dissolving and acid precipitation, and the reaction temperature is controlled at 5-15°C under acidic conditions for diazotization reaction, wherein during the diazotization reaction, sodium nitrite solution is added and then starch potassium iodide test paper is used for detection, until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is carried out, and the reaction is continued for 1 hour, and the starch iodide is kept The potassium chloride test paper has color, and the process uses 2,3 acid as a coupling component, and the dissolved 2,3 acid is coupled with a diazo solution, and the coupling process needs to control the pH value during coupling, and the pH value at the coupling end point is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the end point pH value, and the addition ratio of rosin is 3%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:1;

[0039] S4: Real-time observation: When the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is judged, and the judgment result is processed. If the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and if the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction. If it is judged to be a normal reaction, the reaction is continued. If it is judged to be an abnormal reaction, vaporized pure water is blown into the reaction device through a blower, wherein the temperature of the vaporized pure water is maintained at 5°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the amount of vaporized pure water blown in per unit time is manually increased;

[0040] S5: Customer inspection: The obtained ratio is produced according to the test and samples are sent to customers for inspection. During the inspection, different batches of dry pigments in the ratio table are mixed and crushed according to this ratio, and the final product is tested. The finished product inspection is carried out according to the above inspection method. After the inspection is completed, 100g of finished product samples are sent to the customer for confirmation. The customer will draw the pigment into PP fiber, compare it with the PP fiber made of standard pigment, and judge whether the finished product sample is qualified based on the comparison result. At the same time, the customer will feedback the judgment result. Example 4

[0041] Reference Figure 1 A method for preparing an organic pigment suitable for PP spinning comprises the following steps:

[0042] S1: Method establishment: Professionals establish a pigment inspection method that matches the customer. By using the inspection material polypropylene (PP) that is consistent with the customer, and not using a spinning machine, and using an injection molding machine and a vulcanizer for inspection and color matching, the pigment is first dispersed in polypropylene (PP) at 240°C using an injection molding machine to make a color plate, and the color plates of the standard sample and the test sample prepared at the same time are placed side by side in a vulcanizer to be pressed into a 0.56mm thin sheet. After the pressing is completed, the pressed thin sheet is compared under bright light for color difference, and pigments that match the hiding power, hue and tinting power are selected for adjustment, so that the color difference between the sample and the standard is gradually reduced. At the same time, the transparent color and the surface color need to be considered at the same time to balance the two. The sample obtained in this way is composed of multiple batches of pigments in a certain proportion, not only the strong color, but also the diluted color with the same proportion as the strong color, which is also made into a 0.56mm thin sheet, and the sample is compared with the standard. Through comparison, the tinting power difference is adjusted to be less than or equal to 2%;

[0043] S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin sheets in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and the technician arrives and is Manually perform sheet measurement data feedback, and the technician debugs the vulcanizer based on the feedback data. A pressing test is required for each debugging, and the thickness of the sheet obtained by the pressing test is manually measured, and the thickness measurement result is processed. If the measurement result shows that the sheet thickness data obtained by the pressing test is within the required data range, the vulcanizer is not shut down, and the sheet pressing step is performed. If the measurement result shows that the sheet thickness data obtained by the pressing test is not within the required data range, the vulcanizer is shut down, and the technician continues to debug until the sheet thickness data obtained by the pressing test after debugging is within the required data range, and then the debugging is stopped;

[0044] S3: Adjusting the pigment: Adjusting the pigment production process through diazotization reaction, making the pigment present the hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as the diazo component, and the raw material is formed into fine particles by dissolving and acid precipitation, and the reaction temperature is controlled at 5-15°C under acidic conditions for diazotization reaction, wherein during the diazotization reaction, after adding sodium nitrite solution, starch potassium iodide test paper is used for detection until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is carried out, and the reaction is continued for 1 hour to keep the starch iodide solution. The potassium test paper has color, and the process uses 2,3 acid as a coupling component, and the dissolved 2,3 acid is coupled with a diazo solution, and the coupling process needs to control the pH value during coupling, and the pH value at the coupling end point is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the end point pH value, and the addition ratio of rosin is 2.3%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:1;

[0045] S4: Real-time observation: When the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is judged, and the judgment result is processed. If the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and if the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction. If it is judged to be a normal reaction, the reaction is continued. If it is judged to be an abnormal reaction, vaporized pure water is blown into the reaction device through a blower, wherein the temperature of the vaporized pure water is maintained at 2°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the amount of vaporized pure water blown in per unit time is manually increased;

[0046] S5: Customer inspection: The obtained ratio is produced according to the test and samples are sent to customers for inspection. During the inspection, different batches of dry pigments in the ratio table are mixed and crushed according to this ratio, and the final product is tested. The finished product inspection is carried out according to the above inspection method. After the inspection is completed, 100g of finished product samples are sent to the customer for confirmation. The customer will draw the pigment into PP fiber, compare it with the PP fiber made of standard pigment, and judge whether the finished product sample is qualified based on the comparison result. At the same time, the customer will feedback the judgment result. Example 5

[0047] Reference Figure 1 A method for preparing an organic pigment suitable for PP spinning comprises the following steps:

[0048] S1: Method establishment: Professionals establish a pigment inspection method that matches the customer. By using the inspection material polypropylene (PP) that is consistent with the customer, and not using a spinning machine, and using an injection molding machine and a vulcanizer for inspection and color matching, the pigment is first dispersed in polypropylene (PP) at 260°C using an injection molding machine to make a color plate, and the color plates of the standard sample and the test sample prepared at the same time are placed side by side in a vulcanizer to be pressed into a 0.58mm thin sheet. After the pressing is completed, the pressed thin sheet is compared under bright light for color difference, and pigments that match the hiding power, hue and tinting power are selected for adjustment, so that the color difference between the sample and the standard is gradually reduced. At the same time, the transparent color and the surface color need to be considered at the same time to balance the two. The sample obtained in this way is composed of multiple batches of pigments in a certain proportion, not only the strong color, but also the diluted color in the same proportion as the strong color, which is also made into a 0.58mm thin sheet, and the sample is compared with the standard. By comparison, the tinting power difference is adjusted to be less than or equal to 2%;

[0049] S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin sheets in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and the technician arrives and is Manually perform sheet measurement data feedback, and the technician debugs the vulcanizer based on the feedback data. A pressing test is required for each debugging, and the thickness of the sheet obtained by the pressing test is manually measured, and the thickness measurement result is processed. If the measurement result shows that the sheet thickness data obtained by the pressing test is within the required data range, the vulcanizer is not shut down, and the sheet pressing step is performed. If the measurement result shows that the sheet thickness data obtained by the pressing test is not within the required data range, the vulcanizer is shut down, and the technician continues to debug until the sheet thickness data obtained by the pressing test after debugging is within the required data range, and then the debugging is stopped;

[0050] S3: Adjusting the pigment: Adjusting the pigment production process through diazotization reaction, making the pigment present the hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as the diazo component, and the raw material is formed into fine particles by dissolving and acid precipitation, and the reaction temperature is controlled at 5-15°C under acidic conditions for diazotization reaction, wherein during the diazotization reaction, after adding sodium nitrite solution, starch potassium iodide test paper is used for detection until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is carried out, and the reaction is continued for 1 hour to keep the starch iodide solution. The potassium test paper has color, and the process uses 2,3 acid as a coupling component, and the dissolved 2,3 acid is coupled with a diazo solution, and the coupling process needs to control the pH value during coupling, and the pH value at the coupling end point is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the end point pH value, and the addition ratio of rosin is 2.8%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:1;

[0051] S4: Real-time observation: When the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is judged, and the judgment result is processed. If the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and if the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction. If it is judged to be a normal reaction, the reaction is continued. If it is judged to be an abnormal reaction, vaporized pure water is blown into the reaction device through a blower, wherein the temperature of the vaporized pure water is maintained at 4°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed. If the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the amount of vaporized pure water blown in per unit time is manually increased;

[0052] S5: Customer inspection: The obtained ratio is produced according to the test and samples are sent to customers for inspection. During the inspection, different batches of dry pigments in the ratio table are mixed and crushed according to this ratio, and the final product is tested. The finished product inspection is carried out according to the above method. After the inspection is completed, 100g of finished product samples are sent to the customer for confirmation. The customer will draw the pigment into PP fiber, compare it with the PP fiber made of standard pigment, and judge whether the finished product sample is qualified based on the comparison result. At the same time, the customer will feedback the judgment result.

[0053] The method for preparing an organic pigment suitable for PP spinning in Example 1, Example 2, Example 3, Example 4 and Example 5 was tested, and the results were as follows:

[0054]

[0055] The methods for preparing organic pigments suitable for PP spinning obtained in Examples 1, 2, 3, 4 and 5 have significantly reduced the manufacturing cost of pigments compared to existing methods, and Example 1 is the best example.

[0056] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing an organic pigment suitable for PP spinning, characterized in that: The following steps are involved: S1: Method establishment: Professionals establish pigment inspection methods that match customers; S2: Sampling measurement: Sampling measurement is performed on the thin sheets formed after pressing, and processing is performed based on the measurement results; S3: Adjusting pigments: Adjusting the pigment production process through diazotization reaction and observing the reaction temperature of the reaction process in real time; S4: Real-time observation: During the diazotization reaction, the reaction temperature is manually observed in real time through a temperature detector, and processing is performed based on the observed results; S5: Customer inspection: Produce the obtained ratio according to the test and send samples to the customer for inspection. The inspection determines whether the finished product samples are qualified; In S1, professionals establish a pigment inspection method that matches the customer, by using polypropylene, an inspection material that is consistent with the customer, without using a spinning machine, and using an injection molding machine and a vulcanizing machine for inspection and color matching; When testing and matching colors, first use an injection molding machine to disperse the pigment in polypropylene at 220-300℃ to make a color plate, and place the color plates of the standard sample and the test sample prepared at the same time side by side in a vulcanizer to be pressed into 0.5-0.6mm thin sheets. After pressing, the pressed thin sheets are compared under bright light for color difference, and pigments that match the hiding power, hue and tinting power are selected for adjustment. At the same time, the transparent color and the surface color need to be considered at the same time. It is also necessary to make a diluted color with the same proportion as the strong color, and also make a 0.5-0.6mm thin sheet, and compare the sample with the standard. Through comparison, the tinting power difference is adjusted to be less than or equal to 2%; In S3, the pigment production process is adjusted by diazotization reaction, and the pigment presents a hue and tinting strength consistent with the standard, wherein the pigment uses 2B acid as a diazo component, and the reaction temperature is controlled at 5-15° C. under acidic conditions for diazotization reaction, wherein during the diazotization reaction, sodium nitrite solution is added and then starch potassium iodide test paper is used for detection until the potassium iodide test paper shows blue to complete the detection, and after the detection is completed, stirring is performed and the reaction is continued for 1 hour to keep the starch potassium iodide test paper colored; The process uses 2,3 acid as a coupling component, and couples the dissolved 2,3 acid with a diazo liquid. The coupling process needs to control the pH value during coupling, and the pH value at the coupling endpoint is controlled to be a weakly acidic condition by controlling the pH value during coupling, wherein the weakly acidic condition is pH=4.5, and the desired pigment hue is obtained by adjusting the endpoint pH value, and the addition ratio of rosin is 2-3%, and the pigment hue is adjusted by adjusting the addition amount of calcium chloride and adding strontium chloride, and the ratio of calcium chloride to strontium chloride is 2:

1.

2. The method for preparing an organic pigment suitable for PP spinning according to claim 1, characterized in that: In S2, the thin slices formed after pressing are sampled and measured, wherein the sampling measurement adopts the discontinuous point sampling method for sampling, and there are 50 thin slices in each discontinuous interval, and the thickness is measured manually by using a screw micrometer during the sampling measurement, and the measured thickness data is compared with the required data range, and the comparison result is processed, wherein the comparison result shows that the thickness data measured by the screw micrometer is within the required data range, then the measured thickness data is recorded, and the comparison result shows that the thickness data measured by the screw micrometer is not within the required data range, then the vulcanizer is manually shut down, and a technician is called, and after the technician arrives, the vulcanizer is manually shut down. The technicians will feedback the thin film measurement data, and debug the vulcanizer according to the feedback data. A pressing test is required for each debugging, and the thickness of the thin film obtained from the pressing test is measured manually, and the process is carried out according to the thickness measurement result. If the measurement result is that the thin film thickness data obtained from the pressing test is within the required data range, the vulcanizer will not be shut down, and the thin film pressing step will be carried out. If the measurement result is that the thin film thickness data obtained from the pressing test is not within the required data range, the vulcanizer will be shut down, and the technicians will continue to debug until the thin film thickness data obtained from the pressing test after debugging is within the required data range, and the debugging will be stopped.

3. The method for preparing an organic pigment suitable for PP spinning according to claim 1, characterized in that: In the S4, when the diazotization reaction is carried out, the reaction temperature is manually observed in real time through a temperature detector, and the temperature data obtained by the real-time observation is used for judgment, and the judgment result is processed, wherein the temperature data obtained by the manual real-time observation is within the range of 5-15°C, it is judged as a normal reaction, and the temperature data obtained by the manual real-time observation is not within the range of 5-15°C, it is judged as an abnormal reaction, if it is judged to be a normal reaction, the reaction is continued, if it is judged to be an abnormal reaction, vaporized pure water is blown into the reaction device through a blower, wherein the temperature of the vaporized pure water is maintained at 1-5°C, and after the vaporized pure water is blown in, the real-time observation is continued manually, and the temperature change within 5 minutes after the vaporized pure water is blown in is processed, wherein if the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, no processing is performed, and if the reaction temperature returns to 5-15°C within 5 minutes after the vaporized pure water is blown in, the value of the vaporized pure water blown in per unit time is manually increased.

4. The method for preparing an organic pigment suitable for PP spinning according to claim 1, characterized in that: In S5, the obtained ratio is produced according to the test and samples are sent to the customer for inspection, wherein the inspection is carried out by mixing and crushing different batches of dry pigments in the ratio table according to this ratio, and the final product is tested, wherein the finished product test is carried out according to the above-mentioned test method, after the test is completed, 100g of finished product samples are sent to the customer for confirmation, and the customer reels the pigment into PP fiber, compares it with PP fiber made of standard pigment, and judges whether the finished product sample is qualified through the comparison result, and the customer feedbacks the judgment result.

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