CN115260838B - 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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- CN115260838B CN115260838B CN202211025785.9A CN202211025785A CN115260838B CN 115260838 B CN115260838 B CN 115260838B CN 202211025785 A CN202211025785 A CN 202211025785A CN 115260838 B CN115260838 B CN 115260838B
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/005—Crosslinking of cellulose derivatives
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- 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: preliminary mixing is carried out on the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water according to the weight parts, and the colorant with the corresponding weight parts is slowly added in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water for grinding and stirring, so that the finished pigment is finally obtained. 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 present application relates to the field of pigment manufacturing, and more particularly, to a modified microcrystalline cellulose inorganic pigment and a preparation method thereof.
Background
Inorganic pigments are oxides of nonferrous metals, or metal salts of some metals, and are classified into natural inorganic pigments, which are mineral pigments, and artificial inorganic pigments. Inorganic pigments include various metal oxides, chromates, carbonates, sulfates, sulfides, and the like, such as aluminum powder, copper powder, carbon black, zinc white, titanium white, and the like, all belong to the category of inorganic pigments.
Microcrystalline cellulose is a white, odorless, tasteless crystalline powder composed of finely divided, short, rod-like or powdery porous particles of natural cellulose free flowing to a limited degree of polymerization by hydrolysis with dilute acid. Microcrystalline cellulose can be used as a vehicle for inorganic pigments, so that the dispersibility of inorganic pigments in a substrate is excellent, whereby the dullness of color can be improved. However, the adsorption property of microcrystalline cellulose affects the dispersibility of the inorganic pigment, and microcrystalline cellulose is used as a base material, so that the adsorption property is poor, and the inorganic pigment cannot be stably attached to the microcrystalline cellulose base material.
Disclosure of Invention
In order to improve the adsorption performance of microcrystalline cellulose and improve the dispersibility of inorganic pigment, 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: the 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 colorant, 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 colorant are adopted, so that the colorant can be better adsorbed on modified cellulose crystals, better dispersibility of the pigment is realized, and the modified microcrystalline cellulose is white powder, is nontoxic and odorless and is composed of microcrystals. The characteristic is mainly expressed 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 colorant can be better adsorbed on microcrystalline cellulose, microcrystalline cellulose is commonly used as an adsorbent, the modified microcrystalline cellulose has good adsorption performance, the colorant can be more stably adsorbed on the modified microcrystalline cellulose, and the form of cellulose microparticles comprises microfibers, cellulose crystals, whiskers, single crystals and nanocrystals. The cellulose is subjected to acid hydrolysis under a certain condition, when the polymerization degree is reduced to be in a state of approaching equilibrium, the obtained product is called microcrystalline cellulose, calcium hydroxide provides an alkaline environment for modification of microcrystalline cellulose, so that the cellulose can form gel, the gel has better adsorption performance, the viscosity of silica sol is lower, and water can permeate into places, so that the dispersion and the permeability are very good when the cellulose is mixed with other substances, the colorant is more dispersed and adsorbed on the modified microcrystalline cellulose, the color rendering degree of the pigment is improved, silicone oil is used as an organosilicon defoamer, the silicone defoamer has better defoaming capability, the glossiness and the leveling degree are not easily influenced, the overall color is more uniform, deionized water is used as a solvent, and the colorant is dissolved, so that the colorant can be more easily adsorbed, and the main characteristic effects of better stability, plumpness, uniformity 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 bisacrylamide, 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 grain diameter and large specific surface area, so that the microcrystalline cellulose has special optical properties, rheological properties and mechanical properties, and has chemical functional groups of cellulose, so that hydroxyl groups in the microcrystalline cellulose are main functional groups, and the potential aldehyde groups at the head end can be regarded as functional groups. After the esterification and etherification reactions, the generated esters and ethers have changed mechanical properties, flammability and especially solubility, which greatly increases their applicability. And the microcrystalline cellulose can react with organic matters to form macromolecular oligomers, so that the adsorption performance of the microcrystalline cellulose is improved, the polyvinyl butyral is a product of condensation of polyvinyl alcohol and butyraldehyde under the catalysis of acid, and the microcrystalline cellulose has good flexibility, and can be used as an adsorbent to improve the adsorption performance of the microcrystalline cellulose, so that the pigment is stable. The cross-linking agent N, N-methylene bisacrylamide belongs to a thickening agent and an adhesive of acrylamide, can be used as a cross-linking agent for preparing polyacrylamide gel, and can be cross-linked with microcrystalline cellulose to obtain gel oligomer, so that the adsorption capacity of the microcrystalline cellulose is further improved, and a more stable vehicle is formed through chemical reaction.
Preferably, the modified microcrystalline cellulose comprises the following modification steps:
s1, microcrystalline cellulose is pretreated, microcrystalline cellulose and sulfuric acid aqueous solution with the mass fraction of 0.15% are mixed in a ratio of 1:30g/mL, stirred for 1h at 40 ℃, and subjected to standing filtration, filtrate is taken to be mixed with sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1:10g/mL again, stirred for 1h at 40 ℃, subjected to standing filtration, and filtrate is taken to be washed to be neutral by distilled water, and dried;
s2, N-methylene bisacrylamide is pretreated, and N, N-methylene bisacrylamide is dissolved in ethanol to form a crosslinking agent with the mass fraction of 30%;
s3, mixing the crosslinking agent N, N-methylene bisacrylamide with the mass fraction of 30% 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.
By adopting the technical scheme, microcrystalline cellulose is a polysaccharide compound with small particle size and high crystallinity, the microcrystalline cellulose is mainly composed of a crystallization area in molecules, most of amorphous areas of cellulose raw materials are removed by a biological method or a chemical method to prepare the microcrystalline cellulose, the conventional method for preparing the microcrystalline cellulose is mainly an acid hydrolysis method, beta-1, 4 glycosidic bonds in a cellulose structure are cracked under an acidic condition, the amorphous areas are gradually removed, cellulose molecules are degraded to a limited degree of polymerization to form microcrystalline cellulose, further high-purity cellulose can be prepared, the pretreated microcrystalline cellulose can better form an oligomer, the oligomer can combine the microcrystalline cellulose with polyvinyl butyral by using a cross-linking agent, further the microcrystalline cellulose has good adsorptivity, and N, N-methylenebisacrylamide is dissolved in ethanol by using the cross-linking agent, so that a solution with a certain mass fraction is formed by using the cross-linking agent, further the microcrystalline cellulose is conveniently modified, the functional groups are also conveniently reacted to form a stable oligomer, the microcrystalline cellulose can be better formed into a pigment, the pigment can be combined with the microcrystalline cellulose by using the pretreated microcrystalline cellulose, and the pigment can be sprayed and modified into a microcrystalline cellulose particle, and the pigment can be stably combined with the microcrystalline cellulose.
Preferably, the colorant is an inorganic colorant.
By adopting the above technical scheme, the tinting strength directly determines the dosage of the colorant, generally, as the particle size of the colorant decreases, the inorganic pigment is an oxide of a nonferrous metal or a metal salt insoluble in some metals, and the inorganic pigment is further classified into a natural inorganic pigment and an artificial inorganic pigment, and the natural inorganic pigment is a mineral pigment. 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 10-70 μm.
By adopting the technical scheme, the particle size of the modified microcrystalline cellulose is smaller, so that the pigment is firmly attached to the surface of the fiber, the modified microcrystalline cellulose has stable property and good covering power, and the pigment has good tinting strength.
Preferably, the particle size of the colorant is in the range of 10-60nm.
By adopting the technical scheme, the smaller the particle diameter of the colorant is, the more easily the colorant is adsorbed on the modified microcrystalline cellulose, so that the prepared pigment colorant has high dispersity, the darkness of pigment color is improved, and the aggregation of pigment is inhibited, and meanwhile, the microcrystalline cellulose on the particle surface is soft and has excellent use feeling.
Preferably, the pigment also comprises 3-5 parts by weight of a color fixing agent, wherein the color fixing agent is epichlorohydrin.
According to the technical scheme, the color fixing agent is a cationic surface active quaternary ammonium salt color fixing agent, and the color fixing mechanism is that after the water-soluble anionic dye is dyed, the quaternary ammonium salt with the cation is combined with sulfonic anions on the dye to realize mutual attraction and combination of positive and negative static electricity and generate water-insoluble color lake, so that the color fixing effect is achieved, the color fastness is improved, epoxy chloropropane contains two active atoms and can react with various substances to generate various derivatives. In addition, the epichlorohydrin can be homo-polymerized or copolymerized with other substances to prepare various special-purpose polymer compounds, so that the color fixing effect is better.
In a second aspect, the present application provides a method for preparing a modified microcrystalline cellulose inorganic pigment, which adopts the following technical scheme:
the preparation method of the modified microcrystalline cellulose inorganic pigment comprises the steps of primarily mixing the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water according to the parts by weight, slowly adding the colorant with the 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, and finally obtaining the 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 primarily mixed according to the respective weight parts, so that a space structure with good adsorptivity is formed, the colorant is further more stably adsorbed in the space structure, the colorant and the rest of the deionized water are added for continuous stirring and grinding, namely secondary grinding, so that the dispersibility and the uniformity of a finished product are further improved, the pigment is more in line with the standard of the pigment on the whole, the pigment which meets the quality requirement is continuously and secondarily ground and finally reaches the pigment, the pigment not only has various excellent properties of the previous paint, but also has the auxiliary components of specific types and quantity added in the whole process of transition from the paint to the pigment, and the dispersibility and the uniformity of the finished pigment are further improved.
Preferably, the method further comprises the step of adding a color fixing agent into the pigment, wherein the color fixing agent is epichlorohydrin, and the colorant and the color fixing agent with corresponding parts by weight are slowly added in the preliminary mixing process of the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water for grinding and stirring, so that the finished pigment is finally obtained.
By adopting the above technical solution, the fixing agent is a binder, the purpose of which is to crosslink certain media with each other. The main purpose is to promote molecular chain and accelerating agent of crosslinking, when in use, the agent can be directly added into sizing agent and stirred evenly, or the agent can be firstly hydrated and then added into sizing agent according to the calculated proportion, and stirred evenly. The pigment after the color fixing agent is added, so that the organic substance forms a macromolecular polymer, and the stability of the pigment is improved.
In summary, the present application has the following beneficial effects:
1. since the microcrystalline cellulose crystals and the cross-linking agent are adopted, and the microcrystalline cellulose can react with organic matters to form macromolecular oligomers, so that the adsorption performance of the microcrystalline cellulose is improved, and the cross-linking agent N, N-methylene bisacrylamide belongs to the thickening agent and the binding agent of acrylamide, can be used as the cross-linking agent for preparing polyacrylamide gel, 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 that brightness and pigment color are more bright in the pigment is obtained.
2. The color fixing agent epichlorohydrin is preferably adopted in the application, and 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 homo-polymerized or copolymerized with other substances to prepare various special-purpose high-molecular compounds, and the pigment is more stable.
3. According to the method, the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water are primarily mixed according to the weight parts, so that a space structure with good adsorptivity is formed, the colorant is further stably adsorbed in the space structure, the colorant and the rest of the deionized water are added for continuous stirring and grinding, namely secondary grinding, the dispersibility and the homogeneous phase of a finished product are further improved, and therefore the effects of more stable pigment and brighter color are obtained.
Detailed Description
The following examples are provided to illustrate the present application in further detail, and are specifically described: the following examples, in which no specific conditions are noted, are conducted under conventional conditions or conditions recommended by the manufacturer, and the raw materials used in the following examples are commercially available from ordinary sources except for the specific descriptions.
Microcrystalline cellulose 9004-34-6; the THIS-S30 silica sol; silicone oil PMX200-10CST;
the colorant specifically comprises one of natural cinnabar, laterite, realgar, titanium white, chrome yellow, iron blue, cadmium red, cadmium yellow, lithopone, carbon black, iron oxide red and iron oxide yellow.
Examples of preparation of starting 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, microcrystalline cellulose is pretreated, microcrystalline cellulose and sulfuric acid aqueous solution with the mass fraction of 0.15% are mixed in a ratio of 1:30g/mL, stirred for 1h at 40 ℃, and subjected to standing filtration, filtrate is taken to be mixed with sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1:10g/mL again, stirred for 1h at 40 ℃, subjected to standing filtration, and filtrate is taken to be washed to be neutral by distilled water, and dried;
s2, N-methylene bisacrylamide is pretreated, and N, N-methylene bisacrylamide is dissolved in ethanol to form a crosslinking agent with the mass fraction of 30%;
s3, mixing the crosslinking agent N, N-methylene bisacrylamide with the mass fraction of 30% 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 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, microcrystalline cellulose is pretreated, microcrystalline cellulose and sulfuric acid aqueous solution with the mass fraction of 0.15% are mixed in a ratio of 1:30g/mL, stirred for 1h at 40 ℃, and subjected to standing filtration, filtrate is taken to be mixed with sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1:10g/mL again, stirred for 1h at 40 ℃, subjected to standing filtration, and filtrate is taken to be washed to be neutral by distilled water, and dried;
s2, N-methylene bisacrylamide is pretreated, and N, N-methylene bisacrylamide is dissolved in ethanol to form a crosslinking agent with the mass fraction of 30%;
s3, mixing the crosslinking agent N, N-methylene bisacrylamide with the mass fraction of 30% 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, microcrystalline cellulose is pretreated, microcrystalline cellulose and sulfuric acid aqueous solution with the mass fraction of 0.15% are mixed in a ratio of 1:30g/mL, stirred for 1h at 40 ℃, and subjected to standing filtration, filtrate is taken to be mixed with sulfuric acid aqueous solution with the mass fraction of 0.15% in a ratio of 1:10g/mL again, stirred for 1h at 40 ℃, subjected to standing filtration, and filtrate is taken to be washed to be neutral by distilled water, and dried;
s2, N-methylene bisacrylamide is pretreated, and N, N-methylene bisacrylamide is dissolved in ethanol to form a crosslinking agent with the mass fraction of 30%;
s3, mixing the crosslinking agent N, N-methylene bisacrylamide with the mass fraction of 30% 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.
Examples
Example 1
The preparation method of the modified microcrystalline cellulose inorganic pigment comprises the steps of primarily 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 parts by weight, slowly adding 15kg of colorant 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, and finally obtaining the finished pigment;
the modified microcrystalline cellulose was obtained in preparation example 3.
Example 2
15kg of modified microcrystalline cellulose, 15kg of calcium hydroxide, 5kg of silica sol, 3kg of silicone oil and 80kg of deionized water are primarily mixed according to the weight parts, 25kg of colorant is slowly added 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, and finally the finished pigment is obtained;
the modified microcrystalline cellulose was obtained in preparation example 3.
Example 3
The preparation method of the modified microcrystalline cellulose inorganic pigment comprises the steps of primarily 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 parts by weight, slowly adding 50kg of colorant in the primary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water, and grinding and stirring to finally obtain a finished pigment;
the modified microcrystalline cellulose was obtained 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 colorant and the color fixing agent with corresponding parts by weight in the preliminary mixing process of the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water, and grinding and stirring to finally obtain the finished pigment.
Comparative example
Comparative example 1
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from example 3 in that: modified microcrystalline cellulose is not added to the pigment.
Comparative example 2
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from 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 preparing the same, which are different from example 3 in that: no calcium hydroxide was added to the pigment.
Comparative example 4
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from 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 example 3 in that: the calcium hydroxide in the pigment is replaced with ammonia.
Comparative example 6
A modified microcrystalline cellulose inorganic pigment and a method for preparing the same, which are different from 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 preparing the same, which are different from 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 example 3 in that: the particle size of the colorant ranges from 100 to 200nm.
Performance test
The modified microcrystalline cellulose inorganic pigments obtained in examples 1 to 4 and comparative examples 1 to 8 and the preparation method thereof were respectively taken, and the following performance tests were performed:
dispersion activity: the dispersion degree is reflected by detection, and the particle size is observed by an electron microscope.
Color uniformity: the color difference degree is detected to show that DeltaEab is less than or equal to 1.5 and GB/T5237.5-2000.
Adhesion force: adhesion tester, ISO2409GB/T9286.
The test results are shown in Table 1 below.
TABLE 1
| Project | Dispersion activity | Color uniformity | Adhesion force |
| Example 1 | Good (good) | 0.036 | 0.25 grade |
| Example 2 | Good (good) | 0.034 | 0.25 grade |
| Example 3 | Good (good) | 0.033 | Grade 0.65 |
| Example 4 | Good (good) | 0.031 | Level 0 |
| Comparative example 1 | Difference of difference | 0.081 | Grade 2.00 |
| Comparative example 2 | Difference of difference | 0.069 | 1.50 grade |
| Comparative example 3 | Preferably, it is | 0.072 | 1.85 grade |
| Comparative example 4 | Preferably, it is | 0.066 | Grade 1.25 |
| Comparative example 5 | Difference of difference | 0.074 | Grade 1.05 |
| Comparative example 6 | Preferably, it is | 0.062 | Grade 1.55 |
| Comparative example 7 | Preferably, it is | 0.067 | Grade 1.35 |
| Comparative example 8 | Preferably, it is | 0.071 | Grade 1.45 |
As can be seen from the combination of examples 1 to 4 and comparative examples 1 to 8 and the combination of table 1, example 4 has a relatively good dispersion activity, a relatively high color uniformity and a relatively low adhesion grade, which means that microcrystalline cellulose and polyvinyl butyral can form a macromolecular oligomer by reacting with an organic substance, so that the adsorption performance of microcrystalline cellulose is improved, and a crosslinking agent N, N-methylenebisacrylamide can crosslink with microcrystalline cellulose to obtain a gel oligomer, so that the adsorption capacity of microcrystalline cellulose is further improved, the effect of improving brightness and ensuring a brighter pigment color in a pigment is obtained, and meanwhile, a color fixing agent epichlorohydrin makes the pigment more uniform and stable.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (7)
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 colorant, 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 comprises microcrystalline cellulose, polyvinyl butyral and a cross-linking agent, wherein the cross-linking agent is N, N-methylene bisacrylamide;
the modified microcrystalline cellulose comprises the following modification steps:
s1, preprocessing microcrystalline cellulose, namely mixing microcrystalline cellulose with a sulfuric acid aqueous solution with the mass fraction of 0.15% at the ratio of 1:30g/mL, stirring at 40 ℃ for 1h, standing and filtering, mixing the filtered substance with a sulfuric acid aqueous solution with the mass fraction of 0.15% at the ratio of 1:10g/mL again, stirring at 40 ℃ for 1h, standing and filtering, washing the filtered substance to be neutral by distilled water, and drying;
s2, N-methylene bisacrylamide is pretreated, and N, N-methylene bisacrylamide is dissolved in ethanol to form a crosslinking agent with the mass fraction of 30%;
s3, mixing the crosslinking agent N, N-methylene bisacrylamide with the mass fraction of 30% 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.
2. A modified microcrystalline cellulose inorganic pigment according to claim 1, wherein: the colorant is an inorganic colorant.
3. A modified microcrystalline cellulose inorganic pigment according to claim 1, wherein: the particle size of the modified microcrystalline cellulose ranges from 10 to 70 mu m.
4. A modified microcrystalline cellulose inorganic pigment according to claim 1, wherein: the particle size of the colorant ranges from 10 nm to 60nm.
5. A modified microcrystalline cellulose inorganic pigment according to claim 1, wherein: the pigment also comprises 3-5 parts by weight of a color fixing agent, wherein the color fixing agent is epichlorohydrin.
6. A method of preparing the modified microcrystalline cellulose inorganic pigment of claim 1, wherein: the method comprises the following steps:
preliminary mixing is carried out on the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water according to the weight parts, and the colorant with the corresponding weight parts is slowly added in the preliminary mixing process of the modified microcrystalline cellulose, the calcium hydroxide, the silica sol, the silicone oil and the deionized water for grinding and stirring, so that the finished pigment is finally obtained.
7. The method for producing a modified microcrystalline cellulose inorganic pigment according to claim 6, wherein: and adding a color fixing agent into the pigment, wherein the color fixing agent is epichlorohydrin, slowly adding a colorant and the color fixing agent with corresponding parts by weight in the preliminary mixing process of the modified microcrystalline cellulose, calcium hydroxide, silica sol, silicone oil and deionized water, and grinding and stirring to finally obtain the finished pigment.
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