CN115260838A - Modified microcrystalline cellulose inorganic pigment and preparation method thereof - Google Patents
Modified microcrystalline cellulose inorganic pigment and preparation method thereof Download PDFInfo
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- CN115260838A CN115260838A CN202211025785.9A CN202211025785A CN115260838A CN 115260838 A CN115260838 A CN 115260838A CN 202211025785 A CN202211025785 A CN 202211025785A CN 115260838 A CN115260838 A CN 115260838A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/001—Pigment pastes, e.g. for mixing in paints in aqueous medium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/005—Crosslinking of cellulose derivatives
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
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Abstract
The application relates to the field of pigment manufacturing, and particularly discloses a modified microcrystalline cellulose inorganic pigment and a preparation method thereof. The modified microcrystalline cellulose inorganic pigment comprises the following raw materials: modified microcrystalline cellulose and a colorant, further comprising: calcium hydroxide, silica sol, silicone oil and deionized water; the preparation method comprises the following steps: preliminarily mixing the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water according to respective parts by weight, slowly adding a colorant in a corresponding part by weight in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, grinding and stirring to obtain a finished pigment. The modified microcrystalline cellulose inorganic pigment has the advantage of good dispersibility; in addition, the preparation method has the advantages of simplicity and easiness in operation.
Description
Technical Field
The application relates to the field of pigment manufacturing, in particular to a modified microcrystalline cellulose inorganic pigment and a preparation method thereof.
Background
Inorganic pigments are oxides of nonferrous metals, or some metal-insoluble metal salts, and are further classified into natural inorganic pigments, which are mineral pigments, and artificial inorganic pigments. Inorganic pigments including various metal oxides, chromates, carbonates, sulfates, sulfides, etc., such as aluminum powder, copper powder, carbon black, zinc white, titanium white, etc., are included in the category of inorganic pigments.
Microcrystalline cellulose is white, odorless and tasteless crystalline powder which is formed by hydrolyzing natural cellulose with dilute acid to extremely-fine, free-flowing, short-rod-shaped or powdery porous particles with a limited degree of polymerization. Microcrystalline cellulose can be used as a vehicle for an inorganic pigment, so that the dispersibility of the inorganic pigment in a substrate is excellent, and thus, the dullness of color can be improved. However, the dispersibility of the inorganic pigment is affected by the adsorption performance of the microcrystalline cellulose, and the microcrystalline cellulose serving as a substrate has poor adsorption performance, so that the inorganic pigment cannot be stably attached to the microcrystalline cellulose substrate.
Disclosure of Invention
In order to improve the adsorption performance of microcrystalline cellulose and improve the dispersibility of inorganic pigments, the application provides a modified microcrystalline cellulose inorganic pigment and a preparation method thereof.
In a first aspect, the present application provides a modified microcrystalline cellulose inorganic pigment, which adopts the following technical scheme: a modified microcrystalline cellulose inorganic pigment comprises the following raw materials in parts by weight: 10-20 parts of modified microcrystalline cellulose and 15-50 parts of a coloring agent, and further comprises: 10-30 parts of calcium hydroxide, 2-8 parts of silica sol, 2-5 parts of silicone oil and 50-100 parts of deionized water;
the modified microcrystalline cellulose is obtained by modifying microcrystalline cellulose through N, N-methylene bisacrylamide and polyvinyl butyral.
By adopting the technical scheme, the modified microcrystalline cellulose and the coloring agent are adopted, so that the coloring agent can be better adsorbed on the modified cellulose crystal, and the pigment is better in dispersibility, and the modified microcrystalline cellulose is white powder, is nontoxic and tasteless and consists of microcrystals. The characteristics are mainly shown in the aspects of polymerization degree, crystallization index, grain size and water absorption value, and further can be dissolved in calcium hydroxide, so that the coloring agent can be better adsorbed on microcrystalline cellulose, the microcrystalline cellulose is commonly used as an adsorbent, the modified microcrystalline cellulose has good adsorption performance, the coloring agent can be more stably adsorbed on the modified microcrystalline cellulose, and the cellulose microparticles comprise microfibers, cellulose crystals, whiskers, single crystals and nanocrystals. Cellulose is subjected to acid hydrolysis under certain conditions, when the polymerization degree is reduced to tend to balance, an obtained product is called microcrystalline cellulose, calcium hydroxide provides an alkaline environment for modification of the microcrystalline cellulose, the cellulose can form gel and has better adsorption performance, silica sol has lower viscosity, places where water can permeate, and therefore, the dispersibility and the permeability are very good when the calcium hydroxide is mixed with other substances, a colorant is enabled to be adsorbed on the modified microcrystalline cellulose more dispersedly, the color development degree of the pigment is improved, and silicone oil is used as an organic silicon defoamer, so that the silicon defoamer not only has better defoaming capability, but also is not easy to influence the glossiness and the leveling degree, the whole color is enabled to be fuller and more uniform, deionized water is used as a solvent, the colorant is dissolved, and can be adsorbed more easily, and therefore, the main characteristic effects of better stability, fullness, evenness and the like of a pigment finished product are obtained.
Preferably, the modified microcrystalline cellulose comprises microcrystalline cellulose crystals, polyvinyl butyral and a cross-linking agent, wherein the cross-linking agent is N, N-methylene-bis-acrylamide, and the mass ratio of the microcrystalline cellulose crystals to the cross-linking agent is (85-100): (10-45): (1-15).
By adopting the technical scheme, the microcrystalline cellulose has small particle size and large specific surface area, so that the microcrystalline cellulose has some special optical properties, rheological properties and mechanical properties, the microcrystalline cellulose has a chemical functional group of the cellulose, a hydroxyl group in the microcrystalline cellulose is a main functional group, and a potential aldehyde group at the head end can be regarded as the functional group. After esterification and etherification reactions, the generated esters and ethers have changed mechanical properties, flammability and especially solubility, so that the application properties of the esters and ethers are greatly increased. The polyvinyl butyral is a product obtained by condensing polyvinyl alcohol and butyraldehyde under the catalysis of acid, has good flexibility, can be used as an adsorbent to improve the adsorption performance of the microcrystalline cellulose, and further stabilizes the pigment. The cross-linking agent N, N-methylene bisacrylamide belongs to thickening agents and adhesives of acrylamide, can be used as a cross-linking agent for preparing polyacrylamide gel, can be cross-linked with microcrystalline cellulose to obtain gel oligomers, further improves the adsorption capacity of the microcrystalline cellulose, and further forms a more stable vehicle through chemical reaction.
Preferably, the modified microcrystalline cellulose comprises the following modification steps:
s1, pretreating microcrystalline cellulose, mixing the microcrystalline cellulose with a sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1;
s2, pretreating N, N-methylene bisacrylamide, and dissolving the N, N-methylene bisacrylamide in ethanol to form a cross-linking agent with the mass fraction of 30%;
and S3, mixing 30 mass percent of cross-linking agent N, N-methylene bisacrylamide with the pretreated microcrystalline cellulose particles to obtain slurry, adding polyvinyl butyral into the slurry, and then performing spray drying on the obtained slurry to obtain the modified microcrystalline cellulose.
By adopting the technical scheme, the microcrystalline cellulose is a polysaccharide compound which is formed by glucose units and has small particle size and high crystallinity, the molecule mainly comprises a crystalline region, most amorphous regions of cellulose raw materials are removed by a biological method or a chemical method to prepare the microcrystalline cellulose, the commonly used method for preparing the microcrystalline cellulose at present mainly comprises an acid hydrolysis method, beta-1, 4 glycosidic bonds in the cellulose structure are cracked under an acidic condition, the amorphous regions are gradually removed, cellulose molecules are degraded to a limit polymerization degree to form the microcrystalline cellulose, high-purity cellulose can be further prepared, pretreated microcrystalline cellulose can better form oligomers, the oligomers can combine the microcrystalline cellulose and polyvinyl butyral by using a cross-linking agent, the microcrystalline cellulose has good adsorption, the pretreatment of N, N-methylene bisacrylamide is realized by dissolving N, N-methylene bisacrylamide in ethanol, the cross-linking agent forms a solution with a certain mass fraction, the microcrystalline cellulose can be further conveniently modified, a functional group can be conveniently reacted to form stable oligomers, the obtained colorant can be stably adsorbed, the obtained modified cellulose is dried, and the modified cellulose can be combined with pigment to form pigment particles, so that pigment particles can be prepared.
Preferably, the colorant is an inorganic colorant.
By adopting the technical scheme, the coloring power directly determines the using amount of the coloring agent, generally speaking, the inorganic pigment is an oxide of nonferrous metal or a metal insoluble metal salt, the inorganic pigment is divided into natural inorganic pigment and artificial inorganic pigment, and the natural inorganic pigment is mineral pigment, along with the increase of the particle size of the coloring agent. The pigment has various types, and the dispersibility and the color brightness of the pigment are improved.
Preferably, the modified microcrystalline cellulose has a particle size in the range of 10 to 70 μm.
By adopting the technical scheme, the grain diameter ratio of the modified microcrystalline cellulose is smaller, so that the pigment is firmly attached to the surface of the fiber, and the modified microcrystalline cellulose has stable property, good covering power and good tinting strength.
Preferably, the colorant has a particle size in the range of 10 to 60nm.
By adopting the technical scheme, the smaller the grain diameter of the colorant is, the colorant is easier to be adsorbed on the modified microcrystalline cellulose, so that the prepared pigment colorant has high dispersity, the darkness of the pigment color is improved, the agglomeration of the pigment is inhibited, and the microcrystalline cellulose on the surface of the grain is soft and has excellent use feeling.
Preferably, the pigment also comprises 3-5 parts by weight of a color fixing agent, and the color fixing agent is epichlorohydrin.
By adopting the technical scheme, the color fixing agent is a cationic surface active quaternary ammonium salt color fixing agent, the color fixing mechanism is that after a water-soluble anionic dye is dyed, cationic quaternary ammonium salts are combined with sulfonic anions on the dye to play a role in mutual attraction and combination of positive and negative static electricity to generate water-insoluble color lake, so that the color fixing effect is achieved, the color fastness is improved, and epoxy chloropropane contains two active atoms and can react with various substances to generate various derivatives. In addition, epichlorohydrin can be homopolymerized or copolymerized with other substances to prepare high molecular compounds with various special purposes, so that the color fixing effect is better.
In a second aspect, the present application provides a preparation method of a modified microcrystalline cellulose inorganic pigment, which adopts the following technical scheme:
a modified microcrystalline cellulose inorganic pigment and a preparation method thereof are disclosed, wherein the preparation method comprises the steps of preliminarily mixing the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water according to respective parts by weight, slowly adding a colorant according to the corresponding parts by weight in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, grinding and stirring to finally obtain a finished pigment.
By adopting the technical scheme, the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water are preliminarily mixed according to respective parts by weight to form a spatial structure with good adsorbability, so that the colorant is more stably adsorbed in the spatial structure, the colorant and the rest part of the deionized water are added to continue stirring and grinding, namely secondary grinding, the dispersity and the homogeneity of a finished product are further improved, the pigment integrally better meets the standard of the pigment, the secondary grinding is continued, and finally the pigment meeting the quality requirement is obtained.
Preferably, the method further comprises the step of adding a color fixing agent into the pigment, wherein the color fixing agent is epichlorohydrin, and slowly adding a coloring agent and the color fixing agent in corresponding parts by weight in the primary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water for grinding and stirring to finally obtain the finished pigment.
By adopting the technical scheme, the color fixing agent is an adhesive and aims to crosslink certain media with each other. The main purpose is to promote molecular chain and accelerating cross-linking promoting assistant, when in use, the paste can be directly added and stirred evenly for use, or the paste is added according to the calculated proportion after being hydrated and stirred evenly for use. The pigment added with the color fixing agent enables organic substances to form macromolecular polymers, and the stability of the pigment is improved.
In summary, the present application has the following beneficial effects:
1. because the microcrystalline cellulose crystal and the cross-linking agent are adopted, the microcrystalline cellulose can react with organic matters to form macromolecular oligomers, so that the adsorption performance of the microcrystalline cellulose is improved, the cross-linking agent N, N-methylene bisacrylamide belongs to thickening agents and adhesives of acrylamide, can be used as a cross-linking agent for preparing polyacrylamide gel, and can be cross-linked with the microcrystalline cellulose to obtain gel oligomers, so that the adsorption capacity of the microcrystalline cellulose is further improved, and the effect of improving the brightness and improving the color of the pigment in the pigment is achieved.
2. The dye-fixing agent epichlorohydrin is preferably adopted in the application, the smaller the particle size of the colorant is, the easier the colorant is to be adsorbed on the modified microcrystalline cellulose, so that the prepared pigment colorant has high dispersity, the epichlorohydrin contains two active atoms and can react with various substances to generate various derivatives, the epichlorohydrin can be homopolymerized or copolymerized with other substances to prepare high molecular compounds with various special purposes, and the more stable effect of the pigment is obtained.
3. The method of the application is characterized in that the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water are preliminarily mixed according to respective parts by weight, so that a space structure with good adsorbability is formed, the colorant is adsorbed in the space structure more stably, the colorant and the rest part of the deionized water are added to continue stirring and grinding, namely secondary grinding, the dispersibility and the homogeneity of finished products are further improved, and therefore the effects of more stable pigment and brighter color are obtained.
Detailed Description
The following examples, which are specifically illustrated below, further illustrate the present invention: the following examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer, and the starting materials used in the following examples are available from ordinary commercial sources unless otherwise specified.
Microcrystalline cellulose 9004-34-6; THIS-S30 silica sol; silicone oil PMX200-10CST;
the colorant comprises one of natural cinnabar, red earth, realgar, titanium dioxide, chrome yellow, iron blue, cadmium red, cadmium yellow, lithopone, carbon black, iron oxide red and iron oxide yellow.
Examples of preparation of raw materials and/or intermediates
Preparation example 1
A modified microcrystalline cellulose comprises microcrystalline cellulose crystals and a cross-linking agent, wherein the cross-linking agent is N, N-methylene bisacrylamide, and the mass ratio of the microcrystalline cellulose crystals to the cross-linking agent is 85:10:1.
the method comprises the following modification steps:
s1, pretreating microcrystalline cellulose, mixing the microcrystalline cellulose with a sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1;
s2, pretreating N, N-methylene-bisacrylamide, and dissolving the N, N-methylene-bisacrylamide in ethanol to form a cross-linking agent with the mass fraction of 30%;
and S3, mixing 30 mass percent of cross-linking agent N, N-methylene bisacrylamide with the pretreated microcrystalline cellulose particles to obtain slurry, adding polyvinyl butyral into the slurry, and then performing spray drying on the obtained slurry to obtain the modified microcrystalline cellulose.
Preparation example 2
A modified microcrystalline cellulose comprises microcrystalline cellulose crystals and a cross-linking agent, wherein the cross-linking agent is N, N-methylene-bisacrylamide, and the mass ratio of the microcrystalline cellulose crystals to the cross-linking agent is 90:25:8.
the method comprises the following modification steps:
s1, pretreating microcrystalline cellulose, mixing the microcrystalline cellulose with a sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1;
s2, pretreating N, N-methylene bisacrylamide, and dissolving the N, N-methylene bisacrylamide in ethanol to form a cross-linking agent with the mass fraction of 30%;
s3, mixing 30% by mass of a cross-linking agent N, N-methylene bisacrylamide with the pretreated microcrystalline cellulose particles to obtain slurry, adding polyvinyl butyral into the slurry, and then carrying out spray drying on the obtained slurry to obtain the modified microcrystalline cellulose.
Preparation example 3
A modified microcrystalline cellulose comprises microcrystalline cellulose crystals and a cross-linking agent, wherein the cross-linking agent is N, N-methylene bisacrylamide, and the mass ratio of the microcrystalline cellulose crystals to the cross-linking agent is 100:45:15.
the method comprises the following modification steps:
s1, pretreating microcrystalline cellulose, mixing the microcrystalline cellulose with a sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1;
s2, pretreating N, N-methylene bisacrylamide, and dissolving the N, N-methylene bisacrylamide in ethanol to form a cross-linking agent with the mass fraction of 30%;
and S3, mixing 30 mass percent of cross-linking agent N, N-methylene bisacrylamide with the pretreated microcrystalline cellulose particles to obtain slurry, adding polyvinyl butyral into the slurry, and then performing spray drying on the obtained slurry to obtain the modified microcrystalline cellulose.
Examples
Example 1
A preparation method of a modified microcrystalline cellulose inorganic pigment comprises the steps of preliminarily mixing 10kg of modified microcrystalline cellulose, 10kg of calcium hydroxide, 2kg of silica sol, 2kg of silicone oil and 50kg of deionized water according to the weight parts, slowly adding 15kg of colorant in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, grinding and stirring to obtain a finished pigment;
modified microcrystalline cellulose was obtained as in preparation example 3.
Example 2
A preparation method of a modified microcrystalline cellulose inorganic pigment comprises the steps of preliminarily mixing 15kg of modified microcrystalline cellulose, 15kg of calcium hydroxide, 5kg of silica sol, 3kg of silicone oil and 80kg of deionized water according to the weight parts, slowly adding 25kg of colorant in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, grinding and stirring to obtain a finished pigment;
modified microcrystalline cellulose was obtained as in preparation example 3.
Example 3
A preparation method of a modified microcrystalline cellulose inorganic pigment comprises the steps of preliminarily mixing 20kg of modified microcrystalline cellulose, 30kg of calcium hydroxide, 8kg of silica sol, 5kg of silicone oil and 100kg of deionized water according to the weight parts, slowly adding 50kg of a colorant in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, grinding and stirring to obtain a finished pigment;
modified microcrystalline cellulose was obtained as in preparation example 3.
Example 4
The preparation method of the modified microcrystalline cellulose inorganic pigment further comprises the steps of adding 15kg of a color fixing agent into the pigment, wherein the color fixing agent is epichlorohydrin, slowly adding a coloring agent and the color fixing agent in corresponding parts by weight in the primary mixing process of the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water, grinding and stirring to obtain a finished pigment.
Comparative example
Comparative example 1
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from those of example 3 in that: the pigment was not added with modified microcrystalline cellulose.
Comparative example 2
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from those of example 3 in that: the modified microcrystalline cellulose in the pigment is replaced with microcrystalline cellulose.
Comparative example 3
A modified microcrystalline cellulose inorganic pigment and a method for producing the same, which are different from those of example 3 in that: calcium hydroxide was not added to the pigment.
Comparative example 4
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from those of example 3 in that: no silica sol was added to the pigment.
Comparative example 5
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from those of example 3 in that: the calcium hydroxide in the pigment is replaced by ammonia water.
Comparative example 6
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from those of example 3 in that: the modified microcrystalline cellulose in the pigment is replaced by water-soluble vegetable gum.
Comparative example 7
A modified microcrystalline cellulose inorganic pigment and a method for producing the same, which are different from those of example 3 in that: no silicone oil was added to the pigment.
Comparative example 8
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from those of example 3 in that: the particle size range of the colorant is 100-200nm.
Performance test
The modified microcrystalline cellulose inorganic pigments obtained in examples 1 to 4 and comparative examples 1 to 8 and the preparation methods thereof were respectively subjected to the following performance tests:
dispersing activity: the dispersion degree is detected, and the particle size is observed by using an electron microscope.
Color uniformity: the color difference is detected to show that delta Eab is less than or equal to 1.5, GB/T5237.5-2000.
Adhesion force: adhesion tester, ISO2409GB/T9286.
The test results are shown in table 1 below.
TABLE 1
| Item | Dispersing Activity | Color uniformity | Adhesion force |
| Example 1 | Good taste | 0.036 | Stage 0.25 |
| Example 2 | Good taste | 0.034 | Stage 0.25 |
| Example 3 | Good taste | 0.033 | Grade 0.65 |
| Example 4 | Good taste | 0.031 | Level 0 |
| Comparative example 1 | Difference (D) | 0.081 | Grade 2.00 |
| Comparative example 2 | Difference between | 0.069 | Grade 1.50 |
| Comparative example 3 | Is preferably used | 0.072 | 1.85 stage |
| Comparative example 4 | Is preferably used | 0.066 | Stage 1.25 |
| Comparative example 5 | Difference between | 0.074 | 1.05 grade |
| Comparative example 6 | Is preferably used | 0.062 | 1.55 grade |
| Comparative example 7 | Is preferably used | 0.067 | Grade 1.35 |
| Comparative example 8 | Is preferably used | 0.071 | 1.45 stage |
It can be seen by combining examples 1-4 and comparative examples 1-8 and combining table 1 that example 4 has good dispersion activity, high color uniformity and low adhesion level, which indicates that microcrystalline cellulose and polyvinyl butyral can form macromolecular oligomers through reaction with organic matters, so that the adsorption performance of microcrystalline cellulose is improved, the crosslinking agent N, N-methylene bisacrylamide can be crosslinked with microcrystalline cellulose to obtain gel oligomers, so that the adsorption capacity of microcrystalline cellulose is further improved, the effect of improving brightness and brightening the color of the pigment in the pigment is obtained, and the pigment is more uniform and stable due to the color fixing agent epichlorohydrin.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The modified microcrystalline cellulose inorganic pigment is characterized by comprising the following raw materials in parts by weight: 10-20 parts of modified microcrystalline cellulose and 15-50 parts of a coloring agent, and further comprises: 10-30 parts of calcium hydroxide, 2-8 parts of silica sol, 2-5 parts of silicone oil and 50-100 parts of deionized water;
the modified microcrystalline cellulose is obtained by modifying microcrystalline cellulose with N, N-methylene bisacrylamide and polyvinyl butyral.
2. A modified microcrystalline cellulose inorganic pigment according to claim 1, characterised in that: the modified microcrystalline cellulose comprises microcrystalline cellulose crystals, polyvinyl butyral and a cross-linking agent, wherein the cross-linking agent is N, N-methylene bisacrylamide, and the mass ratio of the microcrystalline cellulose crystals to the cross-linking agent is (85-100): (10-45): (1-15).
3. A modified microcrystalline cellulose inorganic pigment according to claim 1, characterised in that: the modified microcrystalline cellulose comprises the following modification steps:
s1, pretreating microcrystalline cellulose, mixing the microcrystalline cellulose with a sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1;
s2, pretreating N, N-methylene-bisacrylamide, and dissolving the N, N-methylene-bisacrylamide in ethanol to form a cross-linking agent with the mass fraction of 30%;
and S3, mixing 30 mass percent of cross-linking agent N, N-methylene bisacrylamide with the pretreated microcrystalline cellulose particles to obtain slurry, adding polyvinyl butyral into the slurry, and then performing spray drying on the obtained slurry to obtain the modified microcrystalline cellulose.
4. A modified microcrystalline cellulose inorganic pigment according to claim 1, characterised in that: the colorant is an inorganic colorant.
5. A modified microcrystalline cellulose inorganic pigment according to claim 1, characterised in that: the particle size range of the modified microcrystalline cellulose is 10-70 mu m.
6. A modified microcrystalline cellulose inorganic pigment according to claim 1, characterised in that: the particle size range of the colorant is 10-60nm.
7. A modified microcrystalline cellulose inorganic pigment according to claim 1, characterised in that: the pigment also comprises 3-5 parts by weight of a color fixing agent, wherein the color fixing agent is epichlorohydrin.
8. A method for producing a modified microcrystalline cellulose inorganic pigment according to claim 1, characterized in that: the method comprises the following steps:
preliminarily mixing the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water according to respective parts by weight, slowly adding a coloring agent in a corresponding part by weight in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, grinding and stirring to obtain a finished pigment.
9. The method for producing a modified microcrystalline cellulose inorganic pigment according to claim 1, characterized in that: the method comprises the following steps of adding a color fixing agent into the pigment, wherein the color fixing agent is epichlorohydrin, slowly adding a coloring agent and the color fixing agent in corresponding parts by weight in the primary mixing process of the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water, grinding and stirring to finally obtain the finished pigment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05132644A (en) * | 1991-11-12 | 1993-05-28 | Asahi Chem Ind Co Ltd | Inorganic pigment slurry composition |
| JP2018176583A (en) * | 2017-04-14 | 2018-11-15 | スターライト工業株式会社 | Laminate having adhesive reinforcement layer and production method of laminate |
| CN111808466A (en) * | 2020-07-17 | 2020-10-23 | 成都森态源环保科技有限公司 | Anion functional inorganic pigment |
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- 2022-08-25 CN CN202211025785.9A patent/CN115260838B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05132644A (en) * | 1991-11-12 | 1993-05-28 | Asahi Chem Ind Co Ltd | Inorganic pigment slurry composition |
| JP2018176583A (en) * | 2017-04-14 | 2018-11-15 | スターライト工業株式会社 | Laminate having adhesive reinforcement layer and production method of laminate |
| CN111808466A (en) * | 2020-07-17 | 2020-10-23 | 成都森态源环保科技有限公司 | Anion functional inorganic pigment |
Non-Patent Citations (1)
| Title |
|---|
| 刘建平, 东华大学出版社 * |
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