CN113717546A - Method for preparing organic pigment yellow and pigment orange by modifying attapulgite - Google Patents
Method for preparing organic pigment yellow and pigment orange by modifying attapulgite Download PDFInfo
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- CN113717546A CN113717546A CN202111139904.9A CN202111139904A CN113717546A CN 113717546 A CN113717546 A CN 113717546A CN 202111139904 A CN202111139904 A CN 202111139904A CN 113717546 A CN113717546 A CN 113717546A
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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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
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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
- C09B35/00—Disazo and polyazo dyes of the type A<-D->B prepared by diazotising and coupling
- C09B35/02—Disazo dyes
- C09B35/039—Disazo dyes characterised by the tetrazo component
- C09B35/08—Disazo dyes characterised by the tetrazo component the tetrazo component being a derivative of biphenyl
- C09B35/10—Disazo dyes characterised by the tetrazo component the tetrazo component being a derivative of biphenyl from two coupling components of the same type
-
- 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
- C09B35/00—Disazo and polyazo dyes of the type A<-D->B prepared by diazotising and coupling
- C09B35/02—Disazo dyes
- C09B35/039—Disazo dyes characterised by the tetrazo component
- C09B35/08—Disazo dyes characterised by the tetrazo component the tetrazo component being a derivative of biphenyl
- C09B35/10—Disazo dyes characterised by the tetrazo component the tetrazo component being a derivative of biphenyl from two coupling components of the same type
- C09B35/18—Disazo dyes characterised by the tetrazo component the tetrazo component being a derivative of biphenyl from two coupling components of the same type from heterocyclic compounds
-
- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
- C09B67/0007—Coated particulate pigments or dyes with inorganic coatings
Abstract
The method for preparing organic pigment yellow and pigment orange by modifying attapulgite adopts the processed attapulgite to be added into the synthesis process of organic pigment, and comprises four procedures of attapulgite pretreatment, diazo salt preparation, coupling and post-treatment. The pigment particle attapulgite prepared by the process method of the invention is outside, the organic pigment is adsorbed in the attapulgite, and the attapulgite forms a protective layer outside, so that the light fastness and weather resistance of the pigment are greatly improved, the barrier that the light fastness of the organic pigment is limited by the structure of the organic pigment is broken through, simultaneously, each section of the process is optimized, particularly the selection and the control of reaction temperature, and C.I. pigment yellow 12, yellow 14, yellow 65, orange 13 and orange 34 with the characteristics of high light fastness, high weather fastness, high glossiness, high transparency, good fluidity, environmental protection, durability, heat resistance and solvent resistance are produced, so that the pigment particle attapulgite can be widely applied to the fields of automobile and exterior wall decorative coatings, plastic coloring, high-grade ink and the like.
Description
Technical Field
The invention belongs to the technical field of organic pigment application, and particularly relates to a method for preparing organic pigment yellow and pigment orange by attapulgite modification.
Background
The attapulgite is an aqueous magnesium-rich aluminosilicate clay mineral with a layer chain structure, and a layer of magnesium-aluminum-oxygen octahedron is sandwiched between two layers of silicon-oxygen tetrahedrons. The attapulgite is a natural nano silicate material, has high reserves in China, has a nano rod-like microscopic appearance, is usually 30nm in diameter and 300-500 nm in length, and can be widely used for preparing fillers, catalyst carriers, adsorbents, rheology modifiers and material additives for decolorization and desulfurization, sewage treatment, paint auxiliaries and plastic rubber fillers.
The attapulgite with a unique nano rod-shaped structure, a molecular sieve-like microporous structure and surface active silanol groups endows the attapulgite with excellent physicochemical properties such as large specific surface area, strong adsorption capacity, good compatibility and the like. Therefore, the attapulgite is used as a carrier of the temperature-sensitive color-changing compound, so that the weather resistance of the temperature-sensitive hybrid composite pigment to external factors such as acid, alkali, ultraviolet light and the like can be improved, and the thermal stability and the dispersibility and the suspensibility in a water phase system can be improved, thereby expanding the application of the temperature-sensitive hybrid composite pigment in related fields.
Lightfastness refers to the ability of an organic pigment to retain its own color for a specified period of time under solar radiation. This is particularly important for outdoor prints and coatings. Most inorganic pigments and organic pigments, except a few inorganic pigments, undergo more or less discoloration under light. The light fastness of organic pigments is influenced on the one hand by the properties of the organic pigments themselves, including chemical structure and physical form, and on the other hand by the properties of other components in the application system, such as resins, additives, etc. The organic pigment is mainly applied to industries such as coating, printing ink, printing and dyeing, plastic products, papermaking, rubber products, ceramics and the like, and the demand for the pigment is continuously expanded along with the rapid development of downstream industries.
Disclosure of Invention
The invention provides a method for preparing organic pigment yellow and pigment orange by attapulgite modification, which aims to solve the problem that the light fastness and weather fastness of organic pigments cannot be effectively improved under the influence of the properties of the organic pigments and the properties of other components in an application system in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing organic pigment yellow and pigment orange by attapulgite modification comprises four working procedures of attapulgite pretreatment, diazo salt preparation, coupling and post-treatment, and the specific process steps are as follows:
(1) attapulgite pretreatment
A. Grinding
Pulverizing with ball mill or pulverizer, and sieving with 100 mesh, 300 mesh and 400 mesh sieves respectively to obtain attapulgite with fineness of 100 mesh, 300 mesh and 400 mesh;
B. treating the ground attapulgite with acid solution or alkali solution
Adding a certain amount of hydrochloric acid solution with the volume fraction of 32% into the reaction kettle, simultaneously adding a certain amount of distilled water, adding the ground attapulgite, and uniformly stirring for 1-10 hours for later use;
adding a certain amount of liquid caustic soda solution with volume fraction of 32% into a reaction kettle, simultaneously adding a certain amount of distilled water, adding the ground attapulgite, and uniformly stirring for 1-10 hours for later use;
C. pretreating attapulgite with organic solvent or deionized water
Mixing attapulgite and organic solvent with organic solvent such as ethanol, toluene, DMF, etc., treating under azeotropic temperature and reflux for 4-20 hr, or mixing attapulgite and deionized water, reflux treating at about 100 deg.C for 4-50 hr, and filtering;
(2) preparation of diazonium salts
A. Dissolving the diazo component and reacting with sodium nitrite to prepare the diazo liquid
Adding 3000L of water and hydrochloric acid into a diazotization tank, adding 3,3' -dichlorobenzidine hydrochloride or m-nitro-p-anisidine and EDTA while stirring, pulping for 0.5-3 hours, adding ice to cool to below 5 ℃, rapidly adding sodium nitrite solution, controlling the dark blue of potassium iodide test paper, stirring for 30 minutes, adding an auxiliary agent to adjust the light blue of the potassium iodide test paper;
(3) coupling of
A. Dissolving the coupling component under alkaline conditions to obtain a coupling solution:
adding 2000L of water, caustic soda flakes, acetoacetanilide or o-methylacetoacetanilide or o-methoxyacetoacetanilide or 1-phenyl-3-methyl-5-pyrazolone or 1- (p-methylphenyl) -3-methyl-5-pyrazolone and EDTA into a dissolving tank, stirring to dissolve the materials clearly, putting the materials into a coupling tank, adjusting the temperature to be t =15 ℃, adding the prepared attapulgite, adding the dissolved auxiliary agent, controlling the temperature to be t =20 ℃, and waiting for coupling;
B. positive coupling:
adding the treated attapulgite solution into a coupling tank, stirring for 10-60 minutes, adding a diazo component into the coupling tank within 60-120 minutes, ensuring that the pH of the system is =4.0-4.5 and is lower than 4.0 in the dropwise adding process, and adjusting by using dilute alkali liquor, wherein the end point is as follows: pH = 4.0-4.5; the temperature is 10-35 ℃, and the coupling component is in slight excess;
C. inverse coupling:
adding the processed attapulgite solution into a diazo tank, stirring for 10-60 min, adding the coupling component into the diazo tank within 60-120 min, and ensuring the temperature of the system to be below 35 ℃ in the dropwise adding process to obtain the final coupling component in micro-excess;
(4) and (3) post-treatment:
after the coupling reaction is finished, slowly raising the temperature to 70-10 ℃, keeping the temperature for 60-120 minutes, filtering the coupling compound by a pre-pump filter, pumping the coupling compound into a membrane filter press by a slurry pump, carrying out filter pressing for 1.5 hours, adding tap water through a pipeline to rinse the materials to be neutral, then blowing off the materials by compressed air for 10 minutes to form a filter cake, and carrying out wastewater treatment on wastewater generated by filter pressing and rinsing; and (3) drying the filter cake in a belt conveyor for 1-2h, crushing the filter cake in a crusher after drying, putting the crushed filter cake into a mixing barrel, mixing, analyzing, metering and packaging to obtain the C.I. pigment yellow 12, yellow 14, yellow 65, orange 13 or orange 34.
In the step (1), the attapulgite modification is carried out in acid-base or solvent, and the reaction time is 1-10 h.
The assistant added in the step (2) is sulfamic acid, so that the potassium iodide test paper is slightly blue.
In the step (3), the coupling component is dissolved in alkaline conditions to obtain a coupling solution for 1h, and the temperature is controlled at 20 ℃.
The auxiliary agent in the step (3) is one or more surfactants selected from dodecyl guanidine hydrochloride, dodecyl guanidine acetate, octadecyl guanidine hydrochloride, octadecyl guanidine acetate, ethoxylated octadecyl amine guanidine, ethoxylated dodecyl amine guanidine, lauramide guanidine cationic surfactant and dodecyl tetramethyl guanidine cationic surfactant.
The feeding temperature of the filter cake fed into the belt conveyor in the refining process in the step (4) is set to be 80-120 ℃, and the discharging temperature is set to be 60-80 ℃.
And (4) drying the filter cake in the refining process of the step (4) in a belt type machine for 1-2 h.
The technological process of the present invention includes adding treated attapulgite into organic pigment synthesis process to adsorb organic pigment inside attapulgite rod layer structure and to obtain final pigment particle with attapulgite outside, organic pigment adsorbed inside attapulgite rod and protecting layer outside attapulgite rod to raise the light resistance and weather resistance of pigment greatly, break through the limitation of organic pigment structure in light resistance, optimize the technological process, especially the reaction temperature selection and control, and select optimal pigment post-treatment temperature and time to produce C.I. pigment yellow 12, yellow 14, yellow 65, orange 13 and orange 34 with high light fastness, high weather fastness, high brightness, high transparency, high flowability, environment friendship, high heat resistance, high solvent resistance, etc. the technological process of the present invention is suitable for automobile and outer wall decorating paint, plastic coloring, etc High-grade ink and the like.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. Unless otherwise indicated, percentages and parts are weight percentages and kg numbers.
Example 1
Preparation of attapulgite modified organic pigment orange 34
(1) Preparation of diazonium salts
50-100mL of water and 10-15g of hydrochloric acid (30%) are added into a 500mL beaker, 10-20g of 3,3' -dichlorobenzidine hydrochloride (74%) is added with stirring, and the mixture is pulped for 30-60 minutes. Ice is added to reduce the temperature to 0 ℃, and sodium nitrite solution (5.75 g of sodium nitrite (96%) is added into 25mL of water for dissolving) is added at a constant speed within 5 min. Detecting diazo liquid by using starch potassium iodide test paper, wherein the potassium iodide test paper shows blue color, the temperature is less than or equal to 0 ℃, the pH value is less than or equal to 1.5, stirring for 40 minutes, adding sulfamic acid to remove redundant nitrite ions, filtering the diazo liquid, and taking filtrate for later use.
(2) Preparation of coupling liquid
Adding 100-200mL of water into a 2500mL beaker, adding 3-10g (96%) of sodium hydroxide and 10-15g of 1- (p-methylphenyl) -3-methyl-5 pyrazolone under stirring, and stirring and dissolving at 25-28 ℃ until the mixture is clear for coupling.
(3) Synthesis and work-up
Adding the diazo liquid into the coupling liquid under the liquid for 80-90 minutes, and regulating the pH =4.0-4.5 and the temperature T = 20-22 ℃ by using a sodium hydroxide solution in the coupling process. pH =3.5-4.0 after coupling. Stirring for 30min, heating to 90-92 deg.C, and maintaining for 30 min. The temperature is reduced to 65 ℃.
Example 2
Comparative example: the preparation of the diazonium salt, the synthesis of the pigment and the post-treatment are the same as the example 1, 1 to 20g of the processed attapulgite and 0.1 to 1.5 of the auxiliary agent are added in the preparation of the coupling liquid, the temperature rise time of the post-treatment is prolonged, and the heat preservation time is prolonged. And after synthesis, filter pressing and water washing are carried out.
The experimental results are as follows: compared with comparative example 1, the particle size (D50) was larger and the hiding power was slightly lower, but the light fastness and the high weather fastness were improved by one level.
Example 3
Preparation of C.I. pigment yellow 12
(1) Preparation of diazonium salts
50-100mL of water and 10-15g of hydrochloric acid (30%) are added into a 500mL beaker, 10-20g of 3,3' -dichlorobenzidine hydrochloride (74%) is added with stirring, and the mixture is pulped for 30-60 minutes. Ice is added to reduce the temperature to 0 ℃, and sodium nitrite solution (5.75 g of sodium nitrite (96%) is added into 25mL of water for dissolving) is added at a constant speed within 5 min. Detecting diazo liquid by using starch potassium iodide test paper, wherein the potassium iodide test paper shows blue color, the temperature is less than or equal to 0 ℃, the pH value is less than or equal to 1.5, stirring for 40 minutes, adding sulfamic acid to remove redundant nitrite ions, filtering the diazo liquid, and taking filtrate for later use.
(2) Preparation of coupling component and rosin liquid:
preparation of a coupling component: adding 1-10g of sodium hydroxide into 200mL of water with the volume ratio of 100-.
(3) Coupling and post-treatment:
adding the diazo liquid into a coupling tank within 20 minutes, continuously adjusting the pH value with caustic soda flakes, when the pH is =4.1, continuously coupling after adjusting the pH with the caustic soda liquid to be 5.1-5.3, continuously checking the end point with an H-acid solution, keeping the diazo component not excessive, enabling the permeation ring to be colorless, after the coupling is finished, adjusting the pH to be 11.5-12.0 with the caustic soda flakes, heating to 55 ℃, and keeping the temperature for 30 minutes. Adding aluminum sulfate (aluminum sulfate dissolved in water at 60 deg.C), adjusting pH =5-6 (adding a small amount of hydrochloric acid), stirring for 10min, adding water, and cooling to below 50 deg.C.
Example 4
Comparative example: the preparation of the diazonium salt, the synthesis of the pigment and the post-treatment are the same as the example 1, 1 to 20g of the processed attapulgite and 0.1 to 1.5 of the auxiliary agent are added in the preparation of the coupling liquid, the temperature rise time of the post-treatment is prolonged, and the heat preservation time is prolonged. And after synthesis, filter pressing and water washing are carried out.
The experimental results are as follows: compared with comparative example 1, the particle size (D50) was larger and the hiding power was slightly lower, but the light fastness and the high weather fastness were improved by one level.
Example 5
Preparation of c.i. pigment orange 13
(1) Preparation of a diazo component:
adding 15.6g of hydrochloric acid (30%) and 10g of 3,3' -dichlorobenzidine hydrochloride (100%) into 100mL of water, pulping for 60 minutes at room temperature, adding ice to reduce the temperature to-2-0 ℃, rapidly adding sodium nitrite (5.9 g of sodium nitrite (96%) to prepare 30% concentration in advance), and carrying out diazotization reaction at 0-5 ℃, wherein the end point is as follows: changing the potassium iodide starch test paper to blue, stirring for 60 minutes, and regulating the potassium iodide starch test paper to slightly blue by using sulfamic acid to be coupled.
(2) Preparation of coupling component:
adding 3.5g of sodium hydroxide (96%) and 15g of 1-phenyl-3-methyl-5-pyrazolone into 100mL of water, stirring to dissolve, adding 0.3g of red oil, and heating to 32-35 ℃ before coupling.
(3) Coupling and post-treatment:
and (3) putting the diazo component into the coupling liquid for 60min, wherein the pH is = 1.0-1.5 after the coupling is finished, the temperature is 28-30 ℃, and the coupling component is in slight excess. Stirring for 10 minutes, adding the light calcium water soluble slurry, keeping the pH = 1.5-2.0, continuously stirring for 30 minutes, heating to 95 ℃, and keeping the temperature for 20 minutes.
Example 6
Comparative example: the preparation of the diazonium salt, the synthesis of the pigment and the post-treatment are the same as the example 1, 1 to 20g of the processed attapulgite and 0.1 to 1.5 of the auxiliary agent are added in the preparation of the coupling liquid, the temperature rise time of the post-treatment is prolonged, and the heat preservation time is prolonged. And after synthesis, filter pressing and water washing are carried out.
The experimental results are as follows: compared with comparative example 1, the particle size (D50) was larger and the hiding power was slightly lower, but the light fastness and the high weather fastness were improved by one level.
And (3) detecting light fastness and high weather fastness:
the light fastness and high weather fastness of the pigment are generally measured by making a sample into color paste, coating the color paste on a tin plate, placing the tin plate in a light-proof instrument or exposing the tin plate in natural sunlight, and then comparing the color paste with a standard color sample of a blue standard sample card for grading, such as the measuring methods adopted by HGI-456-79 and GB-1710-79.
The determination method comprises the following steps: color paste is prepared according to the same method of the lightfast stability of the pigment in a using medium and is coated on a tin plate.
The method for testing the sunshine resistance instrument comprises the following steps: and (3) shielding half of the prepared tinplate sample plate and the light fastness blue standard sample card by using black thick card paper, placing the tinplate sample plate and the light fastness blue standard sample card in a light-fast instrument, taking out a sample when the tinplate sample plate and the light fastness blue standard sample card are subjected to light until 7 levels of fading (equivalent to 3 levels of a color fastness fading card) in the blue standard sample card are the end point, and grading the sample after the sample plate and the blue standard sample card are placed in a dark place for 30 min.
Comparing the color change degree of the sample with that of a blue standard sample card under scattered light, wherein if the color change degree of the sample is equivalent to a certain grade of the standard sample card, the light fastness of the sample is the grade; if the degree of color change is between two levels, the light fastness is between two levels, with 8 being the best and 1 being the worst.
The test data of the obtained product are shown in the table:
| experiment number | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Light fastness rating | 6 | 7 | 5 | 6 | 5 | 6 |
Note: example 1 and example 2 were compared against comparative example 1; example 3 and example 4 were compared against comparative example 3; example 5 and example 6 were compared against comparative example 5.
Through comparison tests, the pigment obtained by the method has better vividness (delta C); compared with the comparative example, the particle size (D50) is larger, and the light fastness and the high weather fastness are improved by one grade.
The above examples are intended to illustrate the disclosed embodiments of the invention and are not to be construed as limiting the invention. In addition, various modifications of the methods and compositions set forth herein, as well as variations of the methods and compositions of the present invention, will be apparent to those skilled in the art without departing from the scope and spirit of the invention. While the invention has been specifically described in connection with various specific preferred embodiments thereof, it should be understood that the invention should not be unduly limited to such specific embodiments. Indeed, various modifications of the above-described embodiments which are obvious to those skilled in the art to which the invention pertains are intended to be covered by the scope of the present invention.
Claims (7)
1. A method for preparing organic pigment yellow and pigment orange by attapulgite modification is characterized by comprising four working procedures of attapulgite pretreatment, diazonium salt preparation, coupling and post-treatment, and the specific process steps are as follows:
(1) attapulgite pretreatment
A. Grinding
Pulverizing with ball mill or pulverizer, and sieving with 100 mesh, 300 mesh and 400 mesh sieves respectively to obtain attapulgite with fineness of 100 mesh, 300 mesh and 400 mesh;
B. treating the ground attapulgite with acid solution or alkali solution
Adding a certain amount of hydrochloric acid solution with the volume fraction of 32% into the reaction kettle, simultaneously adding a certain amount of distilled water, adding the ground attapulgite, and uniformly stirring for 1-10 hours for later use;
adding a certain amount of liquid caustic soda solution with volume fraction of 32% into a reaction kettle, simultaneously adding a certain amount of distilled water, adding the ground attapulgite, and uniformly stirring for 1-10 hours for later use;
C. pretreating attapulgite with organic solvent or deionized water
Mixing attapulgite and organic solvent with organic solvent such as ethanol, toluene, DMF, etc., treating under azeotropic temperature and reflux for 4-20 hr, or mixing attapulgite and deionized water, reflux treating at about 100 deg.C for 4-50 hr, and filtering;
(2) preparation of diazonium salts
A. Dissolving the diazo component and reacting with sodium nitrite to prepare the diazo liquid
Adding 3000L of water and hydrochloric acid into a diazotization tank, adding 3,3' -dichlorobenzidine hydrochloride or m-nitro-p-anisidine and EDTA while stirring, pulping for 0.5-3 hours, adding ice to cool to below 5 ℃, rapidly adding sodium nitrite solution, controlling the dark blue of potassium iodide test paper, stirring for 30 minutes, adding an auxiliary agent to adjust the light blue of the potassium iodide test paper;
(3) coupling of
A. Dissolving the coupling component under alkaline conditions to obtain a coupling solution:
adding 2000L of water, caustic soda flakes, acetoacetanilide or o-methylacetoacetanilide or o-methoxyacetoacetanilide or 1-phenyl-3-methyl-5-pyrazolone or 1- (p-methylphenyl) -3-methyl-5-pyrazolone and EDTA into a dissolving tank, stirring to dissolve the materials clearly, putting the materials into a coupling tank, adjusting the temperature to be t =15 ℃, adding the prepared attapulgite, adding the dissolved auxiliary agent, controlling the temperature to be t =20 ℃, and waiting for coupling;
B. positive coupling:
adding the treated attapulgite solution into a coupling tank, stirring for 10-60 minutes, adding a diazo component into the coupling tank within 60-120 minutes, ensuring that the pH of the system is =4.0-4.5 and is lower than 4.0 in the dropwise adding process, and adjusting by using dilute alkali liquor, wherein the end point is as follows: pH = 4.0-4.5; the temperature is 10-35 ℃, and the coupling component is in slight excess;
C. inverse coupling:
adding the processed attapulgite solution into a diazo tank, stirring for 10-60 min, adding the coupling component into the diazo tank within 60-120 min, and ensuring the temperature of the system to be below 35 ℃ in the dropwise adding process to obtain the final coupling component in micro-excess;
(4) and (3) post-treatment:
after the coupling reaction is finished, slowly raising the temperature to 70-10 ℃, keeping the temperature for 60-120 minutes, filtering the coupling compound by a pre-pump filter, pumping the coupling compound into a membrane filter press by a slurry pump, carrying out filter pressing for 1.5 hours, adding tap water through a pipeline to rinse the materials to be neutral, then blowing off the materials by compressed air for 10 minutes to form a filter cake, and carrying out wastewater treatment on wastewater generated by filter pressing and rinsing; and (3) drying the filter cake in a belt conveyor for 1-2h, crushing the filter cake in a crusher after drying, putting the crushed filter cake into a mixing barrel, mixing, analyzing, metering and packaging to obtain the C.I. pigment yellow 12, yellow 14, yellow 65, orange 13 or orange 34.
2. The method for preparing organic pigment yellow and pigment orange by attapulgite modification according to claim 1, characterized in that in the step (1), the attapulgite modification is carried out in acid-base or solvent for 1-10 h.
3. The method for preparing organic pigment yellow and pigment orange by modifying attapulgite according to claim 1, which is characterized in that the additive added in the step (2) is sulfamic acid to make potassium iodide test paper bluish.
4. The method for preparing organic pigment yellow and pigment orange by modifying attapulgite according to claim 1, which is characterized in that in the step (3), the coupling component is dissolved under alkaline condition to obtain the coupling liquid for 1h, and the temperature is controlled at 20 ℃.
5. The method for preparing organic pigment yellow and pigment orange by modifying attapulgite according to claim 1, characterized in that the auxiliary agent in the step (3) is one or more surfactants selected from dodecyl guanidine hydrochloride, dodecyl guanidine acetate, octadecyl guanidine hydrochloride, octadecyl guanidine acetate, ethoxylated octadecyl amine guanidine, ethoxylated dodecyl amine guanidine, lauramide guanidine-based cationic surfactant and dodecyl tetramethyl guanidine-based cationic surfactant.
6. The method for preparing organic pigment yellow and pigment orange by attapulgite modification according to claim 1, characterized in that the feeding temperature of the filter cake in the refining process of the step (4) to a belt conveyor is set to be 80-120 ℃, and the discharging temperature is set to be 60-80 ℃.
7. The method for preparing organic pigment yellow and pigment orange by attapulgite modification according to claim 1, characterized in that the drying time of the filter cake in the refining process of the step (4) in a belt type machine is 1-2 h.
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| CN101787220A (en) * | 2010-02-03 | 2010-07-28 | 天津城市建设学院 | Method for preparing natural green nano inorganic material-modified organic pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101787220A (en) * | 2010-02-03 | 2010-07-28 | 天津城市建设学院 | Method for preparing natural green nano inorganic material-modified organic pigment |
| CN102277010A (en) * | 2011-05-05 | 2011-12-14 | 天津城市建设学院 | Preparation method of yellowish scarlet powder subjected to dual modification of core-shell inorganic materials |
| CN102816456A (en) * | 2012-08-29 | 2012-12-12 | 天津城市建设学院 | Method for preparing core pigment red 170 by inorganic nano material modification |
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