CN107083117B - Water-based color paste and preparation method thereof - Google Patents
Water-based color paste and preparation method thereof Download PDFInfo
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- CN107083117B CN107083117B CN201710442637.XA CN201710442637A CN107083117B CN 107083117 B CN107083117 B CN 107083117B CN 201710442637 A CN201710442637 A CN 201710442637A CN 107083117 B CN107083117 B CN 107083117B
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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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- 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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Abstract
The invention discloses aqueous color paste and a preparation method thereof. The aqueous color paste comprises rare earth sulfide pigment, a dispersant, an anti-settling agent and alkaline earth metal oxide serving as a stabilizer. The invention mixes the alkaline earth metal oxide with the rare earth sulfide pigment, thereby improving the stability in water and making the preparation of the aqueous color paste possible. The invention can effectively prevent the rare earth sulfide pigment from settling by being assisted with a dispersant and an anti-settling agent.
Description
Technical Field
The invention relates to an aqueous color paste and a preparation method thereof, in particular to an aqueous color paste containing rare earth compounds and a preparation method thereof.
Background
The red color paste is a mixed paste obtained by adding a filling material and some auxiliary agents into a red pigment. The red pigment includes an organic red pigment and an inorganic red pigment. The organic red pigment has the characteristics of strong tinting strength and good dispersibility; however, they have disadvantages of poor thermal stability and the release of harmful substances such as arylamine and polychlorinated biphenyl. The inorganic red pigment usually contains heavy metal elements such as cadmium, lead, mercury and the like which directly endanger human health and environment. With increasing demands on environmental protection, many countries have strict regulations restricting the use of these pigments. Therefore, a healthy, environment-friendly and stable red color paste product is urgently needed to be found so as to meet the requirements of environmental protection and product performance. The rare earth sulfide red inorganic pigment represented by cerium sulfide has the advantages of both red organic pigment and red inorganic pigment, does not contain heavy metal elements, and is a new generation inorganic pigment substitute which is internationally recognized at present. The red inorganic pigment can replace toxic pigments such as cadmium red, lead red and the like, thereby having great market prospect.
Currently, most rare earth compounds (not usually rare earth sulphide pigments) are applied to colour pastes in the form of rare earth phosphors, such as those disclosed in CN 104695237A. Stability is of little concern because of the very small amounts used. In fact, since the rare earth sulphide pigments have a high specific gravity, the pastes containing them are liable to sedimentation, resulting in a deterioration of their stability. In addition, the stability of the pigment in water is poor, so that it is difficult to prepare an aqueous color paste.
In view of the above, no aqueous color paste containing rare earth sulfide pigment is available at present.
Disclosure of Invention
The inventors of the present application have conducted intensive studies in order to overcome the drawbacks of the prior art, and found that the alkaline earth metal oxide can significantly improve the stability of the rare earth sulfide pigment in water, and that the use of a dispersant in combination with an anti-settling agent can prevent the rare earth sulfide pigment from settling in water.
The invention aims to provide the water-based color paste which has good product stability. A further object of the present invention is an aqueous color paste which does not readily settle.
The invention also aims to provide a preparation method of the water-based color paste, which has simple process and is suitable for large-scale production.
The invention provides an aqueous color paste, which comprises a rare earth sulfide pigment, a dispersant, an anti-settling agent and an alkaline earth metal oxide serving as a stabilizer.
The aqueous color paste according to the invention preferably comprises the following components based on the total weight of the aqueous color paste:
40 to 80 wt% of a rare earth sulfide pigment,
3 to 15 wt% of a dispersant,
2 to 10 wt% of an anti-settling agent, and
0.1 to 3 wt% of an alkaline earth metal oxide.
The aqueous color paste according to the invention preferably further comprises the following components based on the total weight of the aqueous color paste:
0.1 to 3 wt% of a preservative,
3 to 10 wt% of a defoaming agent, and
the balance of water.
The aqueous color paste according to the invention preferably comprises the following components based on the total weight of the aqueous color paste:
40 to 60 wt% of a rare earth sulfide pigment,
3 to 6 wt% of a dispersant,
2 to 5 wt% of an anti-settling agent,
1 to 2 wt% of an alkaline earth metal oxide,
1 to 2 wt% of a preservative,
3 to 6 wt% of a defoaming agent, and
the balance of water.
According to the water-based color paste of the invention, preferably, the rare earth sulfide pigment is Ln2S3Wherein Ln is selected from one or more of lanthanum, cerium, praseodymium, neodymium, samarium, europium or yttrium; and the alkaline earth metal oxide is selected from one or more of calcium oxide, barium oxide or strontium oxide.
According to the water-based color paste disclosed by the invention, preferably, the rare earth sulfide pigment is lanthanum sulfide and/or cerium sulfide; and the alkaline earth metal oxide is calcium oxide.
According to the aqueous color paste disclosed by the invention, preferably, the dispersing agent is selected from an anionic dispersing agent and/or a nonionic dispersing agent; wherein the anionic dispersant is selected from acrylate polymer, higher fatty acid salt, sulfonate, maleic acid-acrylic acid copolymer, styrene-maleic anhydride copolymer, phosphate ester salt or anionic fluorocarbon; the non-ionic dispersing agent is selected from fatty glyceride, fatty sorbitol ester, fatty polyoxyethylene ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, naphthol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alkanolamide polyoxyethylene ether or block copolymer of oxypropylene and oxyethylene; the anti-settling agent is selected from polyurea, polyolefin wax, polyamide wax or fumed silica.
According to the aqueous color paste disclosed by the invention, the preservative is preferably selected from isothiazolinone, p-hydroxybenzoate, sodium benzoate, potassium sorbate or calcium propionate; the defoaming agent is selected from polyether, polyalkylsiloxane and polyether siloxane copolymer emulsion.
According to the water-based color paste disclosed by the invention, preferably, the rare earth sulfide pigment is lanthanum sulfide and/or cerium sulfide; the alkaline earth metal oxide is calcium oxide; the dispersant is acrylate polymer; the anti-settling agent is polyurea; the preservative is isothiazolinone; and the defoaming agent is polyether siloxane copolymer emulsion.
The invention also provides a preparation method of the water-based color paste, which comprises the following steps:
(1) uniformly mixing a dispersing agent, an anti-settling agent, a preservative and water to obtain a dispersion liquid;
(2) slowly adding the rare earth sulfide pigment into the dispersion liquid, stirring for 0.5-2 hours, and grinding for 1-5 hours to obtain pigment slurry;
(3) and adding alkaline earth metal oxide and a defoaming agent into the pigment slurry, defoaming for 0.2-1 hour, and then grinding and filtering to obtain the aqueous color paste.
The invention mixes the alkaline earth metal oxide with the rare earth sulfide pigment, thereby improving the stability of the pigment in water and making the preparation of the aqueous color paste containing the rare earth sulfide pigment possible. The invention can effectively prevent the rare earth sulfide pigment from settling by being assisted with a dispersant and an anti-settling agent. In addition, the color paste obtained according to the preferred technical scheme of the invention has high thixotropy and no fluidity in a static state, but can be recovered to be in a liquid state after being slightly stirred or vibrated; by selecting a proper dispersant, the color paste has excellent fluidity; the color paste is in a pseudo-gel state when in a standing state, cannot easily overflow and leak like liquid, and is convenient to store and transport.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
The percentages of the present invention are expressed in weight percent unless otherwise indicated.
< Water-based color paste >
The aqueous color paste comprises rare earth sulfide pigment, a dispersing agent, an anti-settling agent and alkaline earth metal oxide; preservatives, defoamers, and the like may also be included. In the invention, the alkaline earth metal oxide mainly plays a role of a stabilizer, and can prevent the rare earth sulfide from generating hydrolysis reaction in water so as to influence the stability of the rare earth sulfide. In the invention, the weight percentages of all the components are based on the total weight of the aqueous color paste.
The aqueous color paste of the invention can comprise the following components: 40-80 wt% of rare earth sulfide pigment, 3-15 wt% of dispersing agent, 2-10 wt% of anti-settling agent and 0.1-3 wt% of alkaline earth metal oxide. The aqueous color paste of the invention can also comprise the following components: 0.1-3 wt% of preservative, 3-10 wt% of defoaming agent and the balance of water. In the invention, the amount of water used may be 10 to 70 wt%, preferably 30 to 50 wt%, on the premise of ensuring that the sum of the weight percentages of the components is 100 wt%.
The rare earth sulfide pigment is used in an amount of 40 to 80 wt%, preferably 40 to 60 wt%, and more preferably 40 to 50 wt%. The rare earth sulfide pigment may be Ln2S3Wherein Ln is selected from one or more of lanthanum, cerium, praseodymium, neodymium, samarium, europium or yttrium. The rare earth sulfide pigment can be rare earth sesquisulfide Ln2S3E.g. gamma-Ln2S3. In the invention, Ln is selected from one or more of lanthanum, cerium, praseodymium, neodymium, samarium, europium or yttrium; preferably, Ln is selected from lanthanum or cerium; more preferably, Ln is cerium. According to one embodiment of the present invention, the rare earth sulfide pigment is lanthanum sulfide and/or cerium sulfide.
The alkaline earth metal oxide of the present invention is used in an amount of 0.1 to 3 wt%, preferably 1 to 2 wt%, and more preferably 1 to 1.5 wt%. By controlling the alkaline earth metal oxide in the above range, the stability of the rare earth sulfide pigment in water can be improved, and the influence of the alkaline earth metal oxide on the color of the rare earth sulfide pigment can be reduced. The alkaline earth metal oxide of the present invention may be selected from one or more of calcium oxide, barium oxide or strontium oxide. The alkaline earth metal oxides can very significantly improve the stability of the rare earth sulphide pigments in water. The alkaline earth metal oxide of the present invention is preferably calcium oxide or barium oxide, and is preferably calcium oxide. The invention finds that the calcium oxide has more obvious effect on improving the stability of the rare earth sulfide pigment in water.
The amount of the dispersant is 3 to 15 wt%, preferably 3 to 6 wt%, and more preferably 3 to 3.5 wt%. By controlling the dispersant within the above range, the rare earth sulfide pigment can be prevented from settling in water, and the influence of the dispersant on the color of the rare earth sulfide pigment can be avoided. The dispersant of the present invention may be selected from anionic dispersants and/or nonionic dispersants; anionic dispersants are preferred. The nonionic dispersing agent can be selected from fatty glyceride, fatty sorbitol ester, fatty polyoxyethylene ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, naphthol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alkanolamide polyoxyethylene ether or block copolymer of oxypropylene and oxyethylene; preferably fatty acid polyoxyethylene ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, naphthol polyoxyethylene ether and fatty amine polyoxyethylene ether. The anionic dispersant of the present invention may be selected from acrylate polymers, higher fatty acid salts, sulfonates, maleic acid-acrylic acid copolymers, styrene-maleic anhydride copolymers, phosphate ester salts or anionic fluorocarbons; preferably an acrylate polymer, a maleic acid-acrylic acid copolymer or a styrene-maleic anhydride copolymer. The acrylate polymer includes a copolymer of (meth) acrylate with other comonomers, or a modified polyacrylate polymer. Examples of copolymers of (meth) acrylates with other comonomers include, but are not limited to, those disclosed in CN 105418832A. This patent document discloses only such a dispersion and is used for dispersion of a pigment having good stability in water, for example, carbon black or the like, but does not disclose it for dispersion of a rare earth sulfide pigment having poor stability in water. According to one embodiment of the invention, the dispersant is a modified polyacrylate polymer, which is more beneficial to improve the stability of the rare earth sulfide. Examples of modified polyacrylate polymers include, but are not limited to, DisperSago-9760.
The dosage of the anti-settling agent is 2-10 wt%, preferably 2-5 wt%, and more preferably 2-3 wt%. The anti-settling agent is controlled within the range, so that the rare earth sulfide pigment can be prevented from settling in water, and the influence of the anti-settling agent on the color of the rare earth sulfide pigment is avoided. The anti-settling agent of the present invention may be selected from polyurea, polyolefin wax, polyamide wax or fumed silica; polyurea is preferred. The polyurea of the present invention may be a modified polyurea, specific examples include, but are not limited to, Dispersago-8820.
The amount of the preservative is 0.1 to 3 wt%, preferably 1 to 2 wt%, and more preferably 1 to 1.5 wt%. By controlling the preservative within the above range, the stability of the rare earth sulfide pigment in water can be improved, and the influence of the preservative on the color of the rare earth sulfide pigment can be avoided. The preservatives of the present invention may be selected from isothiazolinone, paraben, sodium benzoate, potassium sorbate or calcium propionate; preferably isothiazolinone or paraben, more preferably isothiazolinone. Examples of preservatives include, but are not limited to, 5-chloro-2-methyl-4-isothiazolin-3-one and/or 2-methyl-4-isothiazolin-3-one. The weight ratio of the two components can be 1-5: 1. The antiseptic can be Rohm and Haas
LXE preservative.
The amount of the defoaming agent is 3 to 10 wt%, preferably 3 to 6 wt%, and more preferably 3 to 3.5 wt%. The defoaming agent is controlled within the range, so that uniform water-based color paste can be obtained, and the influence of the color of the rare earth sulfide pigment on the color of the rare earth sulfide pigment is avoided. The defoaming agent of the present invention is selected from the group consisting of polyethers, polyalkylsiloxanes, polyether siloxane copolymer emulsions; preferably a polyether siloxane copolymer emulsion. Examples of polyether siloxane copolymer emulsions include, but are not limited to, degusside high defoamer Tego Foamex 825.
According to one embodiment of the present invention, the rare earth sulfide pigment is lanthanum sulfide and/or cerium sulfide; the alkaline earth metal oxide is calcium oxide; the dispersant is acrylate polymer; the anti-settling agent is polyurea; the preservative is isothiazolinone; and the defoaming agent is polyether siloxane copolymer emulsion.
< preparation method >
The preparation method of the water-based color paste comprises the following steps: (1) a dispersion liquid preparation step, (2) a pigment slurry preparation step; and (3) forming the aqueous color paste.
The preparation method of the dispersion liquid comprises the step of uniformly mixing the dispersing agent, the anti-settling agent, the preservative and water to obtain the dispersion liquid. The types of the dispersing agent, the anti-settling agent and the preservative, and the using amounts of the dispersing agent, the anti-settling agent, the preservative and the water are not described in detail herein. According to one embodiment of the present invention, the dispersing agent, the anti-settling agent, and the preservative are added to water, and then stirred uniformly to obtain a dispersion liquid.
The preparation method of the pigment slurry comprises the steps of slowly adding the rare earth sulfide pigment into the dispersion liquid, stirring for 0.5-2 hours, and grinding for 1-5 hours to obtain the pigment slurry. In order to avoid agglomeration and the like, the rare earth sulfide pigment needs to be added slowly, for example, the addition is completed within 0.1 to 5 hours, preferably 0.5 to 3 hours. Preferably, stirring is continuously carried out in the adding process, and after all the components are added, high-speed stirring is carried out for 0.5-2 hours, so that uniform dispersion is ensured. Subsequently, the obtained product is ground for 1 to 5 hours, preferably 2 to 3 hours, thereby obtaining a pigment slurry.
The aqueous color paste forming step comprises the steps of adding alkaline earth metal oxide and a defoaming agent into the pigment slurry, defoaming for 0.2-1 hour, and then grinding and filtering to obtain the aqueous color paste. Defoaming was performed under low-speed stirring. The defoaming time is preferably 0.3 to 0.5 hour. Regrinding can further reduce the pigment particle size.
The invention is described in more detail below by way of example.
The cerium sulfide particles are micron-sized solid powder; the calcium oxide is solid powder; the dispersant is Dispersago-9760; the anti-settling agent is Dispergago-8820; the preservative being Rosehas
An LXE preservative; the defoaming agent is degusside high defoaming agentTego Foamex 825。
And (3) viscosity measurement: determined according to the capillary method in GB/T10247-2008.
And (3) determining a sedimentation phenomenon: the method is carried out by visual observation and marked according to the following indexes.
No precipitate is formed;
very small amount of precipitate;
● are precipitated in large amounts.
And (3) measuring the concentration of hydrogen sulfide gas: an MS600 hydrogen sulfide gas detector produced by Shenzhen Yiyuntian electronics Limited company is adopted and measured in the following way. 5g of the aqueous color paste is dispersed in 50g of deionized water and fully mixed by a magnetic stirrer. The container containing the suspension was placed in a 50L airtight box, and then a hydrogen sulfide detector was placed in the airtight box for 24 hours to measure the concentration of hydrogen sulfide gas in the airtight box.
Comparative example 1
Weighing the raw materials according to the formula shown in Table 1, and then preparing the aqueous color paste according to the following steps:
(1) dispersing agent Dispersago-9760, anti-settling agent Dispersago-8820 and preservative
Mixing LXE and water uniformly to obtain a dispersion liquid;
(2) slowly adding rare earth sulfide pigment cerium sulfide particles into the dispersion liquid, stirring for 0.5 hour, and grinding for 2 hours to obtain pigment slurry;
(3) adding a defoaming agent Tego Foamex 825 into the pigment slurry, defoaming for 20 minutes, and then grinding and filtering to obtain the aqueous color paste.
Examples 1 to 3
Weighing the raw materials according to the formula shown in Table 1, and then preparing the aqueous color paste according to the following steps:
(1) dispersing agent Dispersago-9760, anti-settling agent Dispersago-8820 and preservative
LXE and waterUniformly mixing to obtain a dispersion liquid;
(2) slowly adding rare earth sulfide pigment cerium sulfide particles into the dispersion liquid, stirring for 0.5 hour, and grinding for 2 hours to obtain pigment slurry;
(3) adding alkaline earth metal oxide calcium oxide and a defoaming agent Tego Foamex 825 into the pigment slurry, defoaming for 20 minutes, and then grinding and filtering to obtain the aqueous color paste.
TABLE 1 formulation of aqueous color pastes
The viscosities of the aqueous color pastes obtained in examples 1-3 and comparative example 1 were measured by the capillary tube method in GB/T10247-. After 6 months of storage at ambient temperature, the above properties were tested continuously. See table 2 for results. As can be seen from Table 2, the viscosity and tinting strength of the aqueous color pastes obtained in examples 1 to 3 hardly changed, and no significant sedimentation occurred.
TABLE 2 Properties of the aqueous color pastes
| Numbering | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Viscosity, mm2/s | 90 | 95 | 90 | 90 |
| Viscosity after 6 months, mm2/s | 91 | 96 | 92 | 105 |
| Phenomenon of sedimentation | ○ | ○ | ○ | ◎ |
| Sedimentation after 6 months | ○ | ○ | ○ | ● |
| Concentration of hydrogen sulfide ppm | Not detected | Not detected | Not detected | 40 |
| Hydrogen sulfide concentration after 6 months, ppm | Not detected | Not detected | Not detected | 150 |
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (7)
1. The water-based color paste is characterized by comprising the following components based on the total weight of the water-based color paste:
40 to 60 wt% of a rare earth sulfide pigment,
3 to 6 wt% of a dispersant,
2 to 5 wt% of an anti-settling agent,
1 to 2 wt% of an alkaline earth metal oxide,
1 to 2 wt% of a preservative,
3 to 6 wt% of a defoaming agent, and
the balance of water;
wherein, alkaline earth metal oxide is used as a stabilizer; and the alkaline earth metal oxide is calcium oxide.
2. The aqueous color paste according to claim 1, wherein the rare earth sulfide pigment is Ln2S3Wherein Ln is selected from one or more of lanthanum, cerium, praseodymium, neodymium, samarium, europium or yttrium.
3. The aqueous color paste according to claim 2, wherein the rare earth sulfide pigment is lanthanum sulfide and/or cerium sulfide.
4. The aqueous color paste according to any one of claims 1 to 3, which is characterized in that:
the dispersant is selected from anionic dispersant and/or nonionic dispersant; wherein the anionic dispersant is selected from acrylate polymer, higher fatty acid salt, sulfonate, maleic acid-acrylic acid copolymer, styrene-maleic anhydride copolymer, phosphate ester salt or anionic fluorocarbon; the non-ionic dispersing agent is selected from fatty glyceride, fatty sorbitol ester, fatty polyoxyethylene ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, naphthol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alkanolamide polyoxyethylene ether or block copolymer of oxypropylene and oxyethylene;
the anti-settling agent is selected from polyurea, polyolefin wax, polyamide wax or fumed silica.
5. The aqueous color paste according to claim 4, wherein:
the preservative is selected from isothiazolinone, p-hydroxybenzoate, sodium benzoate, potassium sorbate or calcium propionate; and
the defoaming agent is selected from polyether, polyalkylsiloxane and polyether siloxane copolymer emulsion.
6. The aqueous color paste according to claim 5, wherein: the rare earth sulfide pigment is lanthanum sulfide and/or cerium sulfide; the alkaline earth metal oxide is calcium oxide; the dispersant is acrylate polymer; the anti-settling agent is polyurea; the preservative is isothiazolinone; and the defoaming agent is polyether siloxane copolymer emulsion.
7. The preparation method of the water-based color paste according to claim 6, wherein the preparation method comprises the following steps:
(1) uniformly mixing a dispersing agent, an anti-settling agent, a preservative and water to obtain a dispersion liquid;
(2) slowly adding the rare earth sulfide pigment into the dispersion liquid, stirring for 0.5-2 hours, and grinding for 1-5 hours to obtain pigment slurry;
(3) and adding alkaline earth metal oxide and a defoaming agent into the pigment slurry, defoaming for 0.2-1 hour, and then grinding and filtering to obtain the aqueous color paste.
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Effective date of registration: 20180211 Address after: 014000 rare earth building 1807, rare-earth high tech Zone, Baotou, the Inner Mongolia Autonomous Region Applicant after: Baotou Zhongke century science and Technology Co., Ltd. Address before: No. 36 the Yellow River Avenue, Rare Earth Development Zone, Qingshan District, Baotou, the Inner Mongolia Autonomous Region Applicant before: Baotou rare earth research and development center of Chinese Academy of Sciences |
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