CN105038313A - Industrial production method of low-barium environment-friendly lake red pigment 53:1 for plastics - Google Patents
Industrial production method of low-barium environment-friendly lake red pigment 53:1 for plastics Download PDFInfo
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- CN105038313A CN105038313A CN201510417845.5A CN201510417845A CN105038313A CN 105038313 A CN105038313 A CN 105038313A CN 201510417845 A CN201510417845 A CN 201510417845A CN 105038313 A CN105038313 A CN 105038313A
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Abstract
The present invention relates to an industrial production method of a low-barium environment-friendly lake red pigment 53:1 for plastics. Addition of another lake salt for co-lake with barium chloride reduces the amount of introduced barium ions; a sulfate is added for reacting with the free barium ions to generate barium salt, so as to form insoluble barium sulfate; 60 DEG C hot water is used for washing to dissolve and remove barium salt, without affecting the performance of the pigment; and without affecting the tinctorial strength, colored light and vividness, the content of soluble barium salt is effectively controlled at below 100 ppm. The pigment meets the requirements of barium content in coloring agents in EU AP (89) 1 and opens up the market; compared with pigment red 57:1, the pigment provided by the present invention shows more yellow light, has high tinting strength and bright vividness, sensitivity to the pH, good solvent resistance and thermal stability; and the pigment can be applied to the ink, and rubber and plastics, and reaches heat-resistance in HDPE of 260 DEG C / 5min.
Description
Technical field
The present invention relates to a kind of pigment, be specifically related to the industrialized preparing process of a kind of plastic cement with low barium environment-friendly type C lake red CAN'T pigment 53:1.
Background technology
Low barium environment-friendly type C lake red CAN'T pigment 53:1, also claim C.I. Pigment red 53:1, it is a kind of golden light red pigment, and the more aobvious gold-tinted of this pigment ratio Pigment red 57:1, is called warm red, has high tinting strength and vividness, responsive to soda acid.Be applied to ink, there is good solvent resistance and heat-resistant stability; For rubber and plastic cement, heat-resisting 260 DEG C/5min in HDPE.
C.I. Pigment red 53:1 conventional production methods is: after CLT acid, water, liquid caustic soda intensificationization is clear, at low temperatures with hydrochloric acid acid out salify, add sodium nitrite in aqueous solution diazotization, its diazonium salt and coupling component beta naphthal carry out coupled reaction in alkaline medium, again with bariumchloride effect, be transformed into barium salt color lake, thermal treatment, filtration, washing, dry.The C.I. Pigment red 53:1 that makes of this method because of the feed ratio of its CLT acid and bariumchloride be 100:160-180, though to be dissociated barium by aftertreatment and washing part that can be removed, but barium ion content is still at more than 5000ppm in pigment, much larger than the requirement of food safety environment-friendly materials.
Summary of the invention
For the above-mentioned problems in the prior art, the invention provides the industrialized preparing process of a kind of plastic cement with low barium environment-friendly type C lake red CAN'T pigment 53:1.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that comprising the steps:
1) alkali-soluble acid analysis salt-forming reaction: 2-amino-4-methyl-5-chloro Phenylsulfonic acid, water and liquid caustic soda are added in reactor, is warming up to 90-95 DEG C, obtains clear liquor, add concentrated hydrochloric acid in 3-5min, obtain white emulsion, then stir 30min;
2) diazotization reaction: under acidic conditions, adds sodium nitrite in aqueous solution in the white emulsion obtained at 5 DEG C of-10 DEG C of temperature to step 1), obtains diazotization emulsion after carrying out diazotization reaction;
3) add water in coupled reaction still, liquid caustic soda and beta naphthal, stir at 60-65 DEG C of temperature, obtain clear liquor;
4) coupled reaction: under normal temperature (20-25 DEG C), by step 2) the diazotization emulsion that obtains adds in the coupled reaction still of step 3) and carries out coupled reaction, and control reaction system pH in alkalescence, reaction terminates rear stirring 2 hours;
5) color lakeization reaction: add barium chloride solution, stirring reaction in the reaction solution that step 4) obtains; Add another kind of color lake salt brine solution to be again uniformly mixed;
6) pigmenting process: reaction solution step 5) obtained is warming up to 95 DEG C, adds vitriol and stirs cooling, and washing, filtration, dry at 100-120 DEG C, obtain C lake red CAN'T pigment 53:1.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that the 2-amino-4-methyl-5-chloro Phenylsulfonic acid described in step 3) is 100:100-105 with the charged material weight ratio of beta naphthal.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, it is characterized in that couple temperature described in step 4) is at 15-20 DEG C, final pH is at 10-12.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, it is characterized in that the color lake salt described in step 5) and the common color lake of bariumchloride, the feed ratio that 2-amino-4-methyl-5-chloro Phenylsulfonic acid is 100:100-105,2-amino-4-methyl-5-chloro Phenylsulfonic acid and color lake salt with the charged material weight ratio of bariumchloride is 100:60-80.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that the color lake salt described in step 5) is the one in calcium chloride, strontium chloride, manganous sulfate.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that in step 5), churning time is 30-60min; 20-30min is stirred again after adding color lake salt brine solution.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that a kind of vitriol described in step 6) is the one in sodium sulfate, potassium sulfate, magnesium sulfate.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that in step 6), the time, for stirring 30-60min, is cooled to less than 60 DEG C.
Described a kind of plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, it is characterized in that washing warm water in step 6), this warm water temperature is 60 DEG C, to dissolve remaining bariumchloride, adopts diaphragm pressing pressure filter to carry out filter operation.
By adopting above-mentioned technology, compared with prior art, beneficial effect of the present invention is as follows:
The present invention, on the basis of former Pigment red 53:1, by adding another kind of color lake salt and the common color lake of bariumchloride, reduces the introduction volume of barium ion; React generate barium salt by adding a kind of vitriol and free barium, make it generate insoluble barium sulfate; Washing use 60 DEG C of hot water, when not affecting pigment performance, dissolving barium salt, and being removed; When not affecting its tinctorial strength, coloured light and vividness, effectively control the content of soluble barium salt at below 100ppm, meet in European Union AP (89) 1 about barium content requirement in tinting material, open up market, with compared with Pigment red 57:1, the more aobvious gold-tinted of this pigment of the present invention, there is high tinting strength and vividness, responsive to soda acid, by this pigment applications in ink, there is good solvent resistance and heat-resistant stability; For rubber and plastic cement, heat-resisting 260 DEG C/5min in HDPE.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but embodiment does not limit the scope of the invention.
Embodiment 1:
1) diazotization reaction: add in reactor by 228kg2-amino-4-methyl-5-chloro Phenylsulfonic acid, the 1200kg that adds water, liquid caustic soda 155kg, be warming up to 90-95 DEG C, stirs 5min; Add 285kg concentrated hydrochloric acid fast at this temperature, stir 30min; Then slowly add 30% sodium nitrite in aqueous solution 400Kg at 0 DEG C to carry out diazotization reaction and stir 1 hour, excessive Sodium Nitrite thionamic acid removing obtains diazo liquid;
2) coupled reaction: add 1200Kg water in reactor, 220Kg liquid caustic soda, 150Kg2-naphthols, stir, obtain clear liquor at 60 DEG C of temperature; Diazo liquid is injected at 15-20 DEG C this coupled reaction still and carry out coupled reaction, use 5% dilute hydrochloric acid to adjust pH=10.0-10.5, then stir 60min.
3) color lakeization reaction: 125kg bariumchloride is added 400kg water heat up molten clear after, join in this reaction solution, stir 30min, 60kg calcium chloride is added 200kg water stir molten clear after, join in this reaction solution, stir 20min.
4) aftertreatment: this reaction solution is warming up to 95 DEG C, adds 10kg sodium sulfate, stirs 30min, is cooled to 60 DEG C, with 60 DEG C of water washings, pressurization press filtration, dries at 110-120 DEG C.
Embodiment 2
1) diazotization reaction: add in reactor by 228kg2-amino-4-methyl-5-chloro Phenylsulfonic acid, the 1200kg that adds water, liquid caustic soda 155kg, be warming up to 90-95 DEG C, stirs 5min; Add 285kg concentrated hydrochloric acid fast at this temperature, stir 30min; Then slowly add 30% sodium nitrite in aqueous solution 400Kg at 0 DEG C to carry out diazotization reaction and stir 1 hour, excessive Sodium Nitrite thionamic acid removing obtains diazo liquid;
2) coupled reaction: add 1200Kg water in reactor, 220Kg liquid caustic soda, 150Kg2-naphthols, stir, obtain clear liquor at 60 DEG C of temperature; Diazo liquid is injected at 15-20 DEG C this coupled reaction still and carry out coupled reaction, use 5% dilute hydrochloric acid to adjust pH=10-10.5, then stir 60min.
3) color lakeization reaction: 125kg bariumchloride is added 400kg water heat up molten clear after, join in this reaction solution, stir 60min, 80kg strontium chloride is added 200kg water heat up molten clear after, join in this reaction solution, stir 20min.
4) aftertreatment: this reaction solution is warming up to 95 DEG C, adds 10kg sodium sulfate, stirs 60min, is cooled to 50 DEG C, with 60 DEG C of water washings, pressurization press filtration, dries at 110-120 DEG C.
Embodiment 3
1) diazotization reaction: add in reactor by 228kg2-amino-4-methyl-5-chloro Phenylsulfonic acid, the 1200kg that adds water, liquid caustic soda 155kg, be warming up to 90-95 DEG C, stirs 5min; Add 285kg concentrated hydrochloric acid fast at this temperature, stir 30min; Then slowly add 30% sodium nitrite in aqueous solution 400Kg at 0 DEG C to carry out diazotization reaction and stir 1 hour, excessive Sodium Nitrite thionamic acid removing obtains diazo liquid;
2) coupled reaction: add 1200Kg water in reactor, 220Kg liquid caustic soda, 150Kg2-naphthols, stir, obtain clear liquor at 60 DEG C of temperature; Diazo liquid is injected at 15-20 DEG C this coupled reaction still and carry out coupled reaction, use 5% dilute hydrochloric acid to adjust pH=11.0-11.5, then stir 60min.
3) color lakeization reaction: 125kg bariumchloride is added 400kg water heat up molten clear after, join in this reaction solution, stir 60min, 80kg calcium chloride is added 200kg water stir molten clear after, join in this reaction solution, stir 30min.
4) aftertreatment: this reaction solution is warming up to 95 DEG C, adds 10kg potassium sulfate, stirs 30min, is cooled to 50 DEG C, with 60 DEG C of water washings, pressurization press filtration, dries at 110-120 DEG C.
Embodiment 4:
1) diazotization reaction: add in reactor by 228kg2-amino-4-methyl-5-chloro Phenylsulfonic acid, the 1200kg that adds water, liquid caustic soda 155kg, be warming up to 90-95 DEG C, stirs 5min; Add 285kg concentrated hydrochloric acid fast at this temperature, stir 30min; Then slowly add 30% sodium nitrite in aqueous solution 400Kg at 0 DEG C to carry out diazotization reaction and stir 1 hour, excessive Sodium Nitrite thionamic acid removing obtains diazo liquid;
2) coupled reaction: add 1200Kg water in reactor, 220Kg liquid caustic soda, 150Kg2-naphthols, stir, obtain clear liquor at 60 DEG C of temperature; Diazo liquid is injected at 15-20 DEG C this coupled reaction still and carry out coupled reaction, use 5% dilute hydrochloric acid to adjust pH=10-10.5, then stir 60min.
3) color lakeization reaction: 125kg bariumchloride is added 400kg water heat up molten clear after, join in this reaction solution, stir 60min, 80kg strontium chloride is added 200kg water stir molten clear after, join in this reaction solution, stir 30min.
4) aftertreatment: this reaction solution is warming up to 95 DEG C, adds 10kg magnesium sulfate, stirs 60min, is cooled to 60 DEG C, with 60 DEG C of water washings, pressurization press filtration, dries at 110-120 DEG C.
Example related data:
Entrust SGS mechanism to detect, standard is European Union AP (89) 1, uses ICP-OES to analyze, obtains as following table 1 data:
As can be seen from Table 1, the barium ion content in the embodiment of the present invention is all significantly less than limit value.
PVC detection is carried out to pigment, obtains as following table 2 data:
Claims (9)
1. a plastic cement industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that comprising the steps:
1) alkali-soluble acid analysis salt-forming reaction: 2-amino-4-methyl-5-chloro Phenylsulfonic acid, water and liquid caustic soda are added in reactor, is warming up to 90-95 DEG C, obtains clear liquor, add concentrated hydrochloric acid in 3-5min, obtain white emulsion, then stir 30min;
2) diazotization reaction: under acidic conditions, adds sodium nitrite in aqueous solution in the white emulsion obtained at 5 DEG C of-10 DEG C of temperature to step 1), obtains diazotization emulsion after carrying out diazotization reaction;
3) add water in coupled reaction still, liquid caustic soda and beta naphthal, stir at 60-65 DEG C of temperature, obtain clear liquor;
4) coupled reaction: under normal temperature (20-25 DEG C), by step 2) the diazotization emulsion that obtains adds in the coupled reaction still of step 3) and carries out coupled reaction, and control reaction system pH in alkalescence, reaction terminates rear stirring 2 hours;
5) color lakeization reaction: add barium chloride solution, stirring reaction in the reaction solution that step 4) obtains; Add another kind of color lake salt brine solution to be again uniformly mixed;
6) pigmenting process: reaction solution step 5) obtained is warming up to 95 DEG C, adds vitriol and stirs cooling, and washing, filtration, dry at 100-120 DEG C, obtain C lake red CAN'T pigment 53:1.
2. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that the 2-amino-4-methyl-5-chloro Phenylsulfonic acid described in step 3) is 100:100-105 with the charged material weight ratio of beta naphthal.
3. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, it is characterized in that couple temperature described in step 4) is at 15-20 DEG C, final pH is at 10-12.
4. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, it is characterized in that the color lake salt described in step 5) and the common color lake of bariumchloride, the feed ratio that 2-amino-4-methyl-5-chloro Phenylsulfonic acid is 100:100-105,2-amino-4-methyl-5-chloro Phenylsulfonic acid and color lake salt with the charged material weight ratio of bariumchloride is 100:60-80.
5. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that the color lake salt described in step 5) is the one in calcium chloride, strontium chloride, manganous sulfate.
6. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that in step 5), churning time is 30-60min; 20-30min is stirred again after adding color lake salt brine solution.
7. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that a kind of vitriol described in step 6) is the one in sodium sulfate, potassium sulfate, magnesium sulfate.
8. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, is characterized in that in step 6), the time, for stirring 30-60min, is cooled to less than 60 DEG C.
9. a kind of plastic cement according to claim 1 industrialized preparing process of low barium environment-friendly type C lake red CAN'T pigment 53:1, it is characterized in that washing warm water in step 6), this warm water temperature is 60 DEG C, to dissolve remaining bariumchloride, adopts diaphragm pressing pressure filter to carry out filter operation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084882A (en) * | 2016-06-23 | 2016-11-09 | 嘉兴科隆化工有限公司 | A kind of plastic cement industrialized preparing process of low PAHs content safety and environmental protection C lake red CAN'T pigment 53:1 |
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| US6146455A (en) * | 1998-06-19 | 2000-11-14 | Clariant Gmbh | Crystal modification of C.I. Pigment Red 53:2 (δ-phase) |
| CN1803929A (en) * | 2005-12-03 | 2006-07-19 | 青岛大学 | Light resistant, mono azo organic yellow pigment and method for preparing the same |
| CN102585546A (en) * | 2011-12-30 | 2012-07-18 | 山东宇虹颜料有限公司 | Preparation method for C.I. pigment red 53:1 |
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2015
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719292A (en) * | 1982-06-26 | 1988-01-12 | Hoechst Aktiengesellschaft | β-modified crystalline red pigment |
| CN1240219A (en) * | 1998-06-19 | 2000-01-05 | 科莱恩有限公司 | Novel crystal modification of C.I. pigment red 53:2 (gamma-phase) |
| US6146455A (en) * | 1998-06-19 | 2000-11-14 | Clariant Gmbh | Crystal modification of C.I. Pigment Red 53:2 (δ-phase) |
| CN1261614A (en) * | 1998-12-19 | 2000-08-02 | 科莱恩有限公司 | Method for preparing new crystal deformation of C. I. dye red 53 : 2 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106084882A (en) * | 2016-06-23 | 2016-11-09 | 嘉兴科隆化工有限公司 | A kind of plastic cement industrialized preparing process of low PAHs content safety and environmental protection C lake red CAN'T pigment 53:1 |
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Address after: The new road bridge Nanhu District town of Jiaxing City, Zhejiang province 314004 No. 268 Patentee after: CROWN COLOR TECHNOLOGY CO.,LTD. Address before: The new road bridge Nanhu District town of Jiaxing City, Zhejiang province 314004 Jiaxing Kelong Chemical Co. Ltd. Patentee before: CROWN CHEMICAL Co.,Ltd. |
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Denomination of invention: An industrial production method of low barium environment-friendly lake red pigment 53:1 for plastics Effective date of registration: 20230223 Granted publication date: 20170801 Pledgee: Agricultural Bank of China Limited by Share Ltd. South Lake branch Pledgor: CROWN COLOR TECHNOLOGY CO.,LTD. Registration number: Y2023980033346 |
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