CN112175412A - Plastic colorant BK red and preparation method thereof - Google Patents
Plastic colorant BK red and preparation method thereof Download PDFInfo
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- CN112175412A CN112175412A CN202011217948.4A CN202011217948A CN112175412A CN 112175412 A CN112175412 A CN 112175412A CN 202011217948 A CN202011217948 A CN 202011217948A CN 112175412 A CN112175412 A CN 112175412A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B57/00—Other synthetic dyes of known constitution
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/12—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains three hetero rings
- C07D491/14—Ortho-condensed systems
- C07D491/147—Ortho-condensed systems the condensed system containing one ring with oxygen as ring hetero atom and two rings with nitrogen as ring hetero atom
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Abstract
The invention provides a plastic colorant BK red and a preparation method thereof, which are characterized in that: the feed is prepared from the following raw materials in parts by weight: 67-70 parts of hydrochloric acid, 610 parts of water 580-containing alkali, 220 parts of fluorescent red GK 200-containing alkali and 3-5 parts of 30-32% liquid alkali. The method comprises the following specific steps: (1) weighing hydrochloric acid, water and fluorescent red GK according to the parts by weight, sequentially putting the materials into a pulping kettle, and carrying out closed pulping for 13-16 hours at the pulping speed of 2300 plus 2500r/min and the pulping temperature of 35-45 ℃ to obtain a slurry; (2) transferring the slurry prepared in the step (1) to a hydrolysis kettle, heating to 145-155 ℃, carrying out heat preservation reaction for 14-16 hours, and then cooling to 55-65 ℃; (3) transferring the slurry reacted in the step (2) to an alkali treatment kettle, adding liquid alkali to adjust the pH to 7-9, heating to 75-85 ℃, reacting for 1-2 hours, adding water to rinse, filtering, and drying a filter cake at normal pressure and 90-110 ℃ to obtain a finished product. The prepared BK red has high coloring rate, good properties of temperature resistance, solvent resistance and the like, less side reaction and high product purity.
Description
Technical Field
The invention relates to a plastic colorant and a preparation method thereof, in particular to a plastic colorant BK red and a preparation method thereof.
Background
The plastic colorant is used as a raw and auxiliary material in the plastic processing technology, and has the effects of beautifying, decorating, facilitating identification, improving weather resistance, mechanical property, optical property and the like. And are classified into inorganic pigments, organic pigments and dyes. Wherein, pigment means a substance capable of coloring an object. Pigments are distinguished by solubility and insolubility, and by inorganic and organic. The pigment is mainly applied to industries such as coating, printing ink, printing and dyeing, plastic products, papermaking, rubber products, ceramics and the like, the demand for the pigment is continuously expanded along with the rapid development of downstream industries, and the development prospect of the Chinese pigment industry is very wide.
BK Red is solvent Red 196 with a molecular formula of C23H18N4O2The molecular weight is 382.41. The application range is PS, SAN, hard PVC, AS, ABS, PMMA, PET, PBT, PC, PA6, PA66 and other high-end engineering plastics, and the structural formula is shown AS (I): .
Fluorescent colorants themselves often have inherent deficiencies in light and solvent resistance. The coloring rate of BK red on the market is generally 70-80%, the temperature resistance is generally 220 ℃, a plurality of byproducts are produced, the color phase is not good, and the product purity is reduced. Therefore, it is necessary to develop a plastic colorant BK red with high coloring rate, high temperature resistance, good solvent resistance and the like, and can overcome the problems and a preparation method thereof.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the plastic colorant BK red and the preparation method thereof, and the prepared fluorescent red GK has the advantages of high coloring rate, good properties of temperature resistance, solvent resistance and the like, less side reaction and high product purity.
The technical scheme of the invention is realized as follows:
a plastic colorant BK red is prepared from the following raw materials in parts by weight: 67-70 parts of hydrochloric acid, 610 parts of water 580-containing alkali, 220 parts of fluorescent red GK 200-containing alkali and 3-5 parts of 30-32% liquid alkali.
Preferably, the feed is prepared from the following raw materials in parts by weight: 67 parts of hydrochloric acid, 600 parts of water, 210 parts of fluorescent red GK and 3.6 parts of 31% liquid caustic soda.
A preparation method of a plastic colorant BK red comprises the following specific steps:
(1) weighing hydrochloric acid, water and fluorescent red GK according to the parts by weight, sequentially putting the materials into a pulping kettle, and carrying out closed pulping for 13-16 hours at the pulping speed of 2300 plus 2500r/min and the pulping temperature of 35-45 ℃ to obtain a slurry;
(2) transferring the slurry prepared in the step (1) to a hydrolysis kettle, heating to 145-155 ℃, carrying out heat preservation reaction for 14-16 hours, and then cooling to 55-65 ℃;
(3) transferring the slurry reacted in the step (2) to an alkali treatment kettle, adding liquid alkali to adjust the pH to 7-9, heating to 75-85 ℃, reacting for 1-2 hours, adding water to rinse, filtering, and drying a filter cake at normal pressure and 90-110 ℃ to obtain a finished product.
Preferably, the sealing and beating process in the step (1) is carried out at a beating speed of 2400r/min, a beating temperature of 40 ℃ and a beating time of 15 hours.
Preferably, the sealing beating in the step (1) is intermittent beating, and the process is stopped for 10min after 30min of beating.
Preferably, the temperature rising rate in the step (2) is 10-20 ℃/min, and the end point temperature is 150 ℃.
Preferably, the cooling rate in the step (2) is 5-10 ℃/min, and the end point temperature is 60 ℃.
Preferably, the pH is adjusted to 8 by adding liquid alkali in the step (3).
Preferably, in the step (3), the temperature is raised to 80 ℃ for reaction for 1 hour, then water is added for rinsing and filtering, and the filter cake is dried under normal pressure and 100 ℃ to obtain the finished product.
Preferably, the temperature rising rate in the step (3) is 5-15 ℃/min.
The main chemical reactions in the production process are as follows:
the invention has the following beneficial effects: the plastic colorant BK red and the preparation method thereof adopt intermittent pulping, control the pulping speed and temperature to enable heat to be uniformly and rapidly diffused, enable reactants to react uniformly and not to easily generate aggregation, have moderate consistency, are rapid and complete in reaction, have few side reactions and are high in product purity; meanwhile, the corresponding temperature rise speed and temperature are controlled, the product performance is improved, the coloring rate reaches more than 90 percent and is more than 70-80 percent of the coloring rate on the market, the properties of temperature resistance, solvent resistance and the like are good, the main content of the product obtained by high performance liquid chromatography reaches more than 99 percent, and the product has less side reaction and high product purity.
Detailed Description
For a more clear understanding of the technical features, objects and advantages of the present invention, reference is now made to the following detailed description of the embodiments of the present invention taken in conjunction with the accompanying drawings, which are included to illustrate and not to limit the scope of the present invention.
Example 1
A plastic colorant BK red is prepared from the following raw materials in parts by weight: 67 parts of hydrochloric acid, 600 parts of water, 210 parts of fluorescent red GK and 3.6 parts of 31% liquid caustic soda.
A preparation method of a plastic colorant BK red comprises the following specific steps:
(1) weighing hydrochloric acid, water and fluorescent red GK according to parts by weight, sequentially putting into a pulping kettle, sealing and pulping for 15 hours at the pulping speed of 2400r/min and the pulping temperature of 40 ℃, pulping intermittently, and standing for 10min every 30min to obtain a pulp;
(2) transferring the slurry prepared in the step (1) into a hydrolysis kettle, heating to 150 ℃, keeping the temperature, reacting for 15 hours, then cooling to 600 ℃, wherein the heating rate is 10-20 ℃/min, and the cooling rate is 5-10 ℃/min;
(3) transferring the slurry reacted in the step (2) to an alkali treatment kettle, adding liquid alkali to adjust the pH to 8, heating at the rate of 10 ℃/min to 80 ℃, reacting for 1 hour, adding water to rinse, filtering, and drying the filter cake at normal pressure and 100 ℃ to obtain the finished product.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Example 2
A plastic colorant BK red is prepared from the following raw materials in parts by weight: 67 parts of hydrochloric acid, 580 parts of water, 200 parts of fluorescent red GK and 3 parts of 30% liquid alkali.
A preparation method of a plastic colorant BK red comprises the following specific steps:
(1) weighing hydrochloric acid, water and fluorescent red GK according to the parts by weight, sequentially putting into a pulping kettle, sealing and pulping for 13 hours at the pulping speed of 2300r/min and the pulping temperature of 35 ℃, pulping intermittently, and standing for 10min every 30min of pulping to obtain a pulp;
(2) transferring the slurry prepared in the step (1) into a hydrolysis kettle, heating to 145 ℃ at a heating rate of 10 ℃/min, carrying out heat preservation reaction for 14 hours, then cooling to 55 ℃ at a cooling rate of 5 ℃/min;
(3) transferring the slurry reacted in the step (2) to an alkali treatment kettle, adding liquid alkali to adjust the pH to 7, heating at the rate of 5 ℃/min, heating to 75 ℃ to react for 1 hour, adding water to rinse and filter, and drying a filter cake at normal pressure and 90 ℃ to obtain a finished product.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Example 3
A plastic colorant BK red is prepared from the following raw materials in parts by weight: 70 parts of hydrochloric acid, 610 parts of water, 220 parts of fluorescent red GK and 5 parts of 32% liquid alkali.
A preparation method of a plastic colorant BK red comprises the following specific steps:
(1) weighing hydrochloric acid, water and fluorescent red GK according to parts by weight, sequentially putting into a pulping kettle, sealing and pulping for 16 hours at the pulping speed of 2500r/min and the pulping temperature of 45 ℃, pulping intermittently, and standing for 10min after every 30min of pulping to obtain a pulp;
(2) transferring the slurry prepared in the step (1) into a hydrolysis kettle, heating to 155 ℃ at a heating rate of 20 ℃/min, carrying out heat preservation reaction for 16 hours, then cooling to 55 ℃, and cooling at a cooling rate of 10 ℃/min;
(3) transferring the slurry reacted in the step (2) to an alkali treatment kettle, adding liquid alkali to adjust the pH to 9, heating at the rate of 15 ℃/min to 85 ℃, reacting for 2 hours, adding water to rinse, filtering, and drying the filter cake at normal pressure and 110 ℃ to obtain the finished product.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 1
The raw material proportion and the preparation method of the embodiment 1 are selected, the only difference in the preparation method is that the step (1) is not subjected to intermittent pulping, and is directly subjected to continuous pulping, and other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 2
The raw material proportion and the preparation method of the embodiment 1 are selected, the only difference in the preparation method is that the mixture is stopped for 30min after beating in the step (1), and other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 3
The raw material proportion and the preparation method of the embodiment 1 are selected, and the only difference in the preparation method is that the beating speed of the step (1) is 3000r/min, and the beating temperature is 80 ℃. The other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 4
The raw material proportion and the preparation method of the embodiment 1 are selected, and the only difference in the preparation method is that the closed pulping in the step (1) is carried out for 20 hours. The other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 5
The raw material proportion and the preparation method of the embodiment 1 are selected, and the only difference in the preparation method is that the temperature in the step (2) is raised to 200 ℃ and the reaction is carried out for 20 hours under the condition of heat preservation. The other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 6
The raw material ratio and the preparation method of the embodiment 1 are selected, and the only difference in the preparation method is that the temperature of the step (2) is reduced to 40 ℃. The other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 7
The raw material proportion and the preparation method of the embodiment 1 are selected, and the only difference in the preparation method is that the heating rate of the step (2) is 40-50 ℃/min; the other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 8
The raw material proportion and the preparation method of the embodiment 1 are selected, and the only difference in the preparation method is that the cooling rate of the step (2) is 20-30 ℃/min. The other preparation steps are the same.
Comparative example 9
The raw material ratio and the preparation method of the embodiment 1 are selected, the only difference in the preparation method is that the pH value is adjusted to 10 by adding the liquid alkali in the step (3), and other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
Comparative example 10
The raw material ratio and the preparation method of the embodiment 1 are selected, the only difference in the preparation method is that the heating rate of the step (3) is 40 ℃/min, the temperature is increased to 120 ℃ for reaction for 3 hours, and other preparation steps are the same.
And carrying out performance index inspection on the product. The test results are listed in table 1.
First, performance detection
The coloring ratios of the plastic colorants BK red obtained in examples 1 to 3 and comparative examples 1 to 10 and data related to high performance liquid chromatography are shown in Table 1 below.
Solvent resistance: one of the application properties of the pigment is the property of the pigment to resist solvent staining caused by dissolution of the solvent. According to GB/T5211.9-85 pigment solvent resistance test method.
Optical rotation resistance: one of the application properties of the pigment refers to the resistance of the pigment to color change upon exposure to sunlight. According to GB/T1710-79 pigment polarimetry.
TABLE 1
As can be seen from Table 1, the coloring rate (130 ℃, 60min) (mass fraction of dye uptake) of the BK red as a plastic colorant obtained by the method of the present invention is 90% or more, and the BK red is improved in light resistance and solvent resistance and purity as compared with the BK red as a plastic colorant obtained by the above examples and comparative examples. As can be seen from comparative examples 1 to 4, the beating manner, beating temperature, beating speed and beating time in step (1) of the preparation method play an important role in improving the performance of the finished product. As can be seen from comparative examples 5 to 8, the temperature rise rate, the temperature drop rate, the high temperature range, the low temperature range and the reaction time in step (2) of the preparation method have important effects on the performance improvement of the finished product. As can be seen from comparative examples 9 to 10, the pH, the rate of temperature rise, the temperature, etc. in step (3) of the production process play an important role in improving the properties of the finished product.
The above embodiments are merely provided to help understand the method and core principle of the present invention, and the main steps and embodiments of the present invention are described in detail by using specific examples. To those skilled in the art, the various conditions and parameters may be varied as desired in a particular implementation in accordance with the principles of the invention, and in view of the foregoing, the description is not to be taken as limiting the invention.
Claims (10)
1. A plastic colorant BK red, characterized by: the feed is prepared from the following raw materials in parts by weight: 67-70 parts of hydrochloric acid, 610 parts of water 580-containing alkali, 220 parts of fluorescent red GK 200-containing alkali and 3-5 parts of 30-32% liquid alkali.
2. A plastic colorant BK red as claimed in claim 1, wherein: the feed is prepared from the following raw materials in parts by weight: 67 parts of hydrochloric acid, 600 parts of water, 210 parts of fluorescent red GK and 3.6 parts of 31% liquid caustic soda.
3. A method for the preparation of the plastic colorant BK red as claimed in claims 1 to 2, characterized in that: the method comprises the following specific steps:
(1) weighing hydrochloric acid, water and fluorescent red GK according to the parts by weight, sequentially putting the materials into a pulping kettle, and carrying out closed pulping for 13-16 hours at the pulping speed of 2300 plus 2500r/min and the pulping temperature of 35-45 ℃ to obtain a slurry;
(2) transferring the slurry prepared in the step (1) to a hydrolysis kettle, heating to 145-155 ℃, carrying out heat preservation reaction for 14-16 hours, and then cooling to 55-65 ℃;
(3) transferring the slurry reacted in the step (2) to an alkali treatment kettle, adding liquid alkali to adjust the pH to 7-9, heating to 75-85 ℃, reacting for 1-2 hours, adding water to rinse, filtering, and drying a filter cake at normal pressure and 90-110 ℃ to obtain a finished product.
4. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: the sealing beating process in the step (1) is characterized in that the beating speed is 2400r/min, the beating temperature is 40 ℃, and the beating time is 15 hours.
5. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: and (2) in the step (1), the sealed beating is intermittent beating, and the stand is kept for 10min every 30min of beating.
6. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: in the step (2), the heating rate is 10-20 ℃/min, and the end point temperature is 150 ℃.
7. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: the cooling rate in the step (2) is 5-10 ℃/min, and the end point temperature is 60 ℃.
8. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: and (4) adding liquid alkali to adjust the pH value to 8 in the step (3).
9. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: and (3) heating to 80 ℃ in the step (3), reacting for 1 hour, adding water, rinsing, filtering, and drying a filter cake at normal pressure and 100 ℃ to obtain a finished product.
10. A method of producing a plastic colorant BK red as claimed in claim 3, characterized in that: the heating rate in the step (3) is 5-15 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011217948.4A CN112175412A (en) | 2020-11-04 | 2020-11-04 | Plastic colorant BK red and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011217948.4A CN112175412A (en) | 2020-11-04 | 2020-11-04 | Plastic colorant BK red and preparation method thereof |
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| CN202011217948.4A Pending CN112175412A (en) | 2020-11-04 | 2020-11-04 | Plastic colorant BK red and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3880869A (en) * | 1972-11-02 | 1975-04-29 | Basf Ag | Dyes of the benzopyrane series |
| JPH06316881A (en) * | 1993-05-06 | 1994-11-15 | Nippon Kayaku Co Ltd | Sheet for heat-sensitive transfer |
| JPH06316649A (en) * | 1993-05-06 | 1994-11-15 | Nippon Kayaku Co Ltd | Method for coloring organic high-molecular material using benzopyran compound |
-
2020
- 2020-11-04 CN CN202011217948.4A patent/CN112175412A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3880869A (en) * | 1972-11-02 | 1975-04-29 | Basf Ag | Dyes of the benzopyrane series |
| JPH06316881A (en) * | 1993-05-06 | 1994-11-15 | Nippon Kayaku Co Ltd | Sheet for heat-sensitive transfer |
| JPH06316649A (en) * | 1993-05-06 | 1994-11-15 | Nippon Kayaku Co Ltd | Method for coloring organic high-molecular material using benzopyran compound |
Non-Patent Citations (3)
| Title |
|---|
| 冉兴: ""香豆素荧光分散染料的合成研究"", 《大连理工大学硕士学位论文》 * |
| 智双等: "香豆素类染料的荧光光谱性能及应用性能研究 ", 《染料与染色》 * |
| 高本春等: "香豆素系高档荧光溶剂染料合成工艺 ", 《染料工业》 * |
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Application publication date: 20210105 |