TW202229375A - Dispersion and ink - Google Patents

Abstract

A dispersion includes 100 parts by weight of powder, 1 to 80 parts by weight of dispersant, and 80 to 900 parts by weight of polar solvent. The dispersant is a diblock copolymer having a chemical structure of, wherein Ini and Ini' are residue groups of an initiator of polymerization, each of R1 is independently H or methyl group, R2, B is alkali metal or N(R3)4, and each of R3 is independently H, C1-4 alkyl group, or C1-4 hydroxyalkyl group; m and n have a ratio of 3:1 to 1:2, and x is 0.7 to 1. The dispersant has a weight average molecular weight (Mw) of 1500 to 4500.

Description

Dispersions and Inks

The present disclosure pertains to dispersions and inks, and more particularly to the dispersants employed therein.

Micropowder dispersion technology is widely used in digital inkjet printing inks and coatings. There is a large market demand for dispersants used to disperse organic/inorganic micropowders, especially polymer dispersants used in aqueous dispersions that meet environmental protection requirements. Aqueous dispersions can be combined with resins to form water-based inks, and their advantages include safety, non-toxicity, harmlessness, and almost no volatile organic gas generation, so the development of dispersants is extremely important. The dispersant plays a key role in the technology of stabilizing the dispersion of conductive carbon black with high conductivity. To achieve the above goals, it is urgent to design the structure of the aqueous dispersant for micropowders.

，其中Ini與Ini’係聚合反應所用之起始劑的殘基；每一R ¹各自為H或甲基；R ²係

、

、或

；B係鹼金族金屬或N(R ³) ₄，且每一R ³各自為H、C _1-4的烷基、或C _1-4的烷基醇，m與n的比例為3:1至1:2；以及x係0.7至1，其中該分散劑的重量平均分子量(Mw)為1500至4500。 A dispersion liquid provided by an embodiment of the present disclosure includes: 100 parts by weight of powder; 1 to 80 parts by weight of a dispersant; and 80 to 900 parts by weight of a polar solvent, wherein the dispersant is a double-block copolymer, which is The chemical structure is:

, wherein Ini and Ini' are the residues of the initiators used in the polymerization reaction; each R ¹ is independently H or methyl; R ² is

,

,or

; B is an alkali metal group or N(R ³ ) ₄ , and each R ³ is independently H, a C _1-4 alkyl group, or a C _1-4 alkyl alcohol, and the ratio of m to n is 3: 1 to 1:2; and x is 0.7 to 1, wherein the weight average molecular weight (Mw) of the dispersant is 1500 to 4500.

，其中Ini與Ini’係聚合反應所用之起始劑的殘基；每一R ¹各自為H或甲基；R ²係

、

、或

；B係鹼金族金屬或N(R ³) ₄，且每一R ³各自為H、C _1-4的烷基、或C _1-4的烷基醇，m與n的比例為3:1至1:2；x係0.7至1，其中分散劑的重量平均分子量(Mw)為1500至4500。 An ink provided by an embodiment of the present disclosure includes: a dispersion liquid and a resin, and the weight ratio of the dispersion liquid to the resin is 100:10 to 100:120, wherein the dispersion liquid includes: 100 parts by weight of powder; 1 to 80 parts by weight dispersant; and 80 to 900 parts by weight of polar solvent, wherein the dispersant is a double block copolymer, and its chemical structure is:

, wherein Ini and Ini' are the residues of the initiators used in the polymerization reaction; each R ¹ is independently H or methyl; R ² is

,

,or

; B is an alkali metal group or N(R ³ ) ₄ , and each R ³ is independently H, a C _1-4 alkyl group, or a C _1-4 alkyl alcohol, and the ratio of m to n is 3: 1 to 1:2; x is 0.7 to 1, wherein the weight average molecular weight (Mw) of the dispersant is 1500 to 4500.

A dispersion liquid provided in an embodiment of the present disclosure includes: 100 parts by weight of powder; 1 to 80 parts by weight of dispersant; and 80 to 900 parts by weight of polar solvent. If the proportion of the dispersant is too low, the powder cannot be effectively dispersed. If the proportion of the dispersant is too high, the cost will be increased instead, if the powder cannot be further dispersed. Furthermore, if the dispersion is subsequently used in the ink, an excessively high proportion of the dispersant can affect the coating properties (eg, conductivity) formed by the ink. If the ratio of the polar solvent is too low, the powder is easily precipitated. If the proportion of polar solvent is too high, the practicality of the product will be reduced.

。Ini與Ini’係聚合反應所用之起始劑的殘基。舉例來說，若採用原子轉移自由基聚合(ATRP)的聚合機制，則Ini可為C ₁-C ₁₂脂肪族烷基、C ₆-C ₁₂芳香族烷基、或一般市售的ATRP起始劑的殘基，而Ini’可為Cl或Br。若採用其他聚合機制如陽離子型聚合或陰離子型聚合，則Ini與Ini’可為對應的殘基。每一R ¹各自為H或甲基；R ²係

、

、或

；B係鹼金族金屬或N(R ³) ₄，且每一R ³各自為H、C _1-4的烷基、或C _1-4的烷基醇。m與n的比例為3:1至1:2。若m的比例過低且n的比例過高，則分散劑不易溶於水。若m的比例過高且n的比例過低，則分散劑不易吸附粉體。x係0.7至1。舉例來說，可中和大部分的酸基(x=0.7)，或將所有的酸基中和(x=1)。上述分散劑的重量平均分子量(簡稱重均分子量)為1500至4500。若分散劑的重均分子量過低，則分散劑不易吸附粉體。若分散劑的重均分子量過高，則無法有效分散粉體。若分散劑為無規共聚物，則無法有效分散粉體。 The aforementioned dispersant is a double block copolymer, and its chemical structure is:

. Residues of initiators used in the polymerization reaction of Ini and Ini'. For example, if the polymerization mechanism of atom transfer radical polymerization (ATRP) is employed, Ini can be initiated by _C1 - _C12 aliphatic alkyl, _C6 - _C12 aromatic alkyl, or commonly commercially available ATRP Residue of the agent, and Ini' can be Cl or Br. If other polymerization mechanisms such as cationic or anionic polymerization are employed, Ini and Ini' may be corresponding residues. Each R ¹ is independently H or methyl; R ² is

,

,or

; B is an alkali metal or N(R ³ ) ₄ , and each R ³ is independently H, a C _1-4 alkyl group, or a C _1-4 alkyl alcohol. The ratio of m to n is 3:1 to 1:2. If the ratio of m is too low and the ratio of n is too high, the dispersant is not easily soluble in water. If the ratio of m is too high and the ratio of n is too low, the dispersant will not easily adsorb the powder. x is 0.7 to 1. For example, most of the acid groups can be neutralized (x=0.7), or all acid groups can be neutralized (x=1). The weight-average molecular weight (abbreviated as weight-average molecular weight) of the above-mentioned dispersant is 1,500 to 4,500. If the weight-average molecular weight of the dispersant is too low, the dispersant is unlikely to adsorb powder. If the weight average molecular weight of the dispersant is too high, the powder cannot be effectively dispersed. If the dispersant is a random copolymer, the powder cannot be effectively dispersed.

In one embodiment, the synthesis method of the above dispersant is as follows. It should be noted that the following methods are only used as examples rather than limitations of the present disclosure. The above-mentioned dispersants can be synthesized by those of ordinary skill in the art using available equipment and pharmaceuticals.

First, tertiary butyl acrylate ( tBMA ) can be taken with an initiator (Initiator, such as p-methylphenylsulfonyl chloride) to form a polymer, as shown below. In the following formula, Ini can be _CH3 -Ph- _SO2- , and Ini' can be -Cl.

Another acrylate after deoxygenation, such as isobutyl methacrylate ( iBMA ), is then added to the above polymer and reacted to form a biblock copolymer. It can be understood that since the two monomer systems of tBMA and iBMA react sequentially rather than simultaneously, the resulting copolymer is a biblock copolymer rather than a random copolymer. The above-mentioned polymerization mechanism is ATRP, and its reaction is as follows:

The block corresponding to m is then deprotected with acid, and the deprotected copolymer is optionally neutralized as follows:

In the above reaction, the definitions of Ini, Ini', R ¹ , R ² , m, n, x, and B are the same as those described above, and will not be repeated here.

In some embodiments, the aforementioned powders include carbon materials, pigments, metals, metal oxides, or combinations thereof. For example, the carbon material may include carbon black, graphite, graphene, carbon nanotubes, fullerenes, or other suitable carbon materials, or a combination thereof. Pigments can be yellow pigments such as cadmium yellow (PY35, C.I.77205, CAS# 12237-67-1), titanium nickel yellow (PY53, C.I.77788, CAS#8007-18-9), zirconium yellow (PY159, C.I.77997, CAS#68187-15-5), Chrome Titanium Yellow (PY162, C.I.77896, CAS#68611-42-7; PY163, C.I.77897, CAS# 68186-92-5), or Bismuth Yellow (PY184, C.I.771740, CAS #14059-33-7). Pigments can be magenta pigments such as iron red (PR101, C.I.77491, CAS# 1317-60-8), cadmium red (PR108, C.I.77202, CAS#58339-34-7), lead chrome red (PR104, C.I.77605, CAS#12656-85-8; PR105, C.I.77578, CAS#1314-41-6), or iron zirconium red (PR232, C.I.77996, CAS#68412-79-3). Pigments can be cyan pigments such as cobalt blue (PB28, C.I. 77364, CAS# 68187-40-6) and cobalt chrome blue (PB36, C.I. 77343, CAS# 68187-11-1). Pigments can be black pigments such as manganese iron black (PBK26, C.I.77494, CAS# 68186-94-7; PBK33, C.I.77537, CAS #75864-23-2), cobalt iron chrome black (PBK27, C.I.77502, CAS#68186 -97-0), Copper Chrome Black (PBK28, C.I.77428, CAS#68186-91-4), Chrome Iron Black (PBK30, C.I.77504, CAS#71631-15-7), or Titanium Black (PBK35, C.I.77890 , CAS# 70248-09-8). Pigments can be white inorganic pigments such as titanium white (PW6, C.I.77891, CAS#13463-67-7), zirconium white (PW12, C.I.77990, CAS#1314-23-4), or zinc white (PW4, C.I.77947, CAS#1314-13-2). Pigments can be orange pigments such as cadmium orange (PO20, C.I.77199, CAS#12656-57-4) and chrome orange (PO21, C.I.77601, CAS#1344-38-3). Pigments can be green pigments such as chrome green (PG17, C.I.77288, CAS#1308-38-9), cobalt green (PG19, C.I.77335, CAS#8011-87-8), cobalt chrome green (PG26, C.I.77344, CAS #68187-49-5), or Cobalt Titanium Green (PG50, C.I.77377, CAS#68186-85-6). The pigment may also be other suitable pigments, not limited to the above-mentioned pigments.

In some embodiments, the average particle size of the powder may be 100 nm to 550 nm, such as 100 nm to 350 nm. Generally speaking, the smaller the average particle size of the pigment powder, the better. In addition, when the above-mentioned dispersion liquid is stored at room temperature for more than half a year, the particle size of the powder can still be maintained without significant change, which shows that the above-mentioned dispersion liquid has excellent stability. In some embodiments, the aforementioned polar solvents include water, diethylene glycol diethyl ether, diethylene glycol dimethyl ether, propylene glycol methyl ether acetate, diethylene glycol butyl ether acetate, ethylene glycol butyl ether, tetrakis Glycol dimethyl ether, or a combination of the above.

An ink provided by an embodiment of the present disclosure includes: the above-mentioned dispersion liquid and a resin, and the weight ratio of the dispersion liquid to the resin is 100:10 to 100:120. The resin may include polypropylene resin, polyurethane resin, or a combination of the above. If the ratio of the resin is too low, the powder adhesion will deteriorate. If the proportion of resin is too high, the powder properties are not easily exhibited. For example, commercially available adhesives such as VSR-50 (available from Dow Chemical), ESP-2293 (available from ESP materials), SP3901 (available from Chichi Chemical), and 2026c (available from Liuhe Chemical) and The dispersions are mixed to form the ink. In some embodiments, the powder in the ink has an average particle size of 100 nm to 550 nm. Generally speaking, if the average particle size of the powder in the ink is much larger than the average particle size of the powder in the dispersion, it means that the dispersant has poor compatibility with the resin. In some embodiments, the difference between the average particle size of the powder in the ink and the average particle size of the powder in the dispersion may be less than 5%.

In order to make the above-mentioned content and other objects, features, and advantages of the present disclosure more obvious and easy to understand, preferred embodiments are given below, and are described in detail as follows in conjunction with the accompanying drawings: [Example]

In the following examples, the measurement methods of the powder particle size in the dispersion liquid or ink, such as _Dave , D ₉₅ , and D ₁₀₀ , are ISO-13320 standard methods.

Synthesis Example 1 (DBDI-01) After dissolving N,N,N',N',N''- pentamethyldiethylenetriamine (PMDETA, 7.90 g, 45.59 mmole) in tetrahydrofuran (THF, 65 mL), Nitrogen was bubbled through the THF solution to remove oxygen. Then CuBr (6.54 g, 45.59 mmole) was added to the solution and stirred well. Then CuBr ₂ (2.04 g, 9.12 mmole) was added to the THF solution and stirred well.

Tertiary butyl methacrylate (tBMA, 77.80 g, 547.12 mmole) and p-methylphenylsulfonyl chloride ( p -TsCl, 8.69 g, 45.59 mmole) were dissolved in THF (65 mL) and purged with nitrogen into THF solution to deoxygenate. After this solution was added to the PMDETA solution, the above reactants were heated to 40°C under nitrogen for about 18 hours to form PtBMA . The above-mentioned polymerization mechanism is atom transfer radical polymerization (ATRP), and its reaction is as follows:

Nitrogen gas was introduced into isobutyl methacrylate ( iBMA , 77.80 g, 547.12 mmole) to deoxygenate, then the deoxygenated iBMA was added to the PtBMA solution, and the above reaction was heated to 40 °C under nitrogen to react for about At 24 hours, the bi-block copolymer PtBMA - b - PiBMA was formed. It can be understood that since the two monomer systems of tBMA and iBMA react sequentially rather than simultaneously, the resulting copolymer is a biblock copolymer rather than a random copolymer. The above-mentioned polymerization mechanism is ATRP, and its reaction is as follows:

After the above-mentioned reaction is cooled, the crude product solution after the above-mentioned reaction is filtered with a neutral alumina column, and the filtrate is reprecipitated with n-hexane, and a white solid (P t BMA- b -P i BMA) is collected. The Mw of the above-mentioned product is about is 6600, Mn is 4300, and PDI is 1.5. In the above formula, m=10, n=19.

Next, PtBMA - b - PiBMA (100 g, 23.25 mmol) and dioxane (120 mL) were mixed and stirred under nitrogen, and then hydrochloric acid (11.0 mL, 128 mmol) was added to the above mixture, and heated to The reaction was carried out at 85°C for 18 hours. After cooling the reaction, the solvent was removed by concentration. After dissolving the crude product in THF until it has low viscosity and fluidity, the insoluble matter is filtered off. The solution was then added to n-hexane for reprecipitation, and the filter cake was collected by filtration. After drying the filter cake, a white solid PMAA- b -P i BMA (acid value of about 200-215 mg KOH/g) was obtained. PMAA- b -P i BMA has Mw=4900, Mn=2700, and PDI=1.8. Next, 60 g of PMAA- b -P i BMA powder was stirred and dispersed in 267 mL of deionized water, and a 28% ammonia solution (14.9 g) was dropped into the above dispersion, and then heated to 70 °C for 5 hours. After completely dissolving, the pH value of the above solution was adjusted to above 8 with ammonia water to obtain double-block copolymer DBDI-01 (solid content: 18.2 wt%). The above reaction is as follows:

Synthesis Example 2 (DBDI-02) After PMDETA (7.90 g, 45.59 mmole) was dissolved in THF (65 mL), nitrogen gas was passed through the THF solution to deoxygenate. Then CuBr (6.54 g, 45.59 mmole) was added to the solution and stirred well. Then CuBr ₂ (2.04 g, 9.12 mmole) was added to the THF solution and stirred well.

tBMA (77.80 g, 547.12 mmole) and p -TsCl (8.69 g, 45.59 mmole) were dissolved in THF (65 mL) and nitrogen was bubbled through the THF solution to deoxygenate. Then, after adding this solution to the PMDETA solution, the above reactants were heated to 40°C under nitrogen for 18 hours to form PtBMA . The above-mentioned polymerization mechanism is atom transfer radical polymerization (ATRP), and its reaction is as follows:

Nitrogen gas was introduced into iBMA (38.90 g, 273.56 mmole) to deoxygenate, then the deoxygenated iBMA was added to the PtBMA solution, and the above reaction was heated to 40 °C under nitrogen for 24 hours to form double clumps Copolymer PtBMA - b - PiBMA . It can be understood that since the two monomer systems of tBMA and iBMA react sequentially rather than simultaneously, the resulting copolymer is a biblock copolymer rather than a random copolymer. The above-mentioned polymerization mechanism is ATRP, and its reaction is as follows:

After the above reaction was cooled, the crude product solution after the above reaction was filtered with a neutral alumina column, and the filtrate was reprecipitated with n-hexane, and a white solid (P t BMA- b -P i BMA) was collected. The above product had a Mw of 3800, a Mn of 2500, and a PDI of 1.5. In the above formula, m=10, n=6.

Next, PtBMA - b - PiBMA (70 g, 28.00 mmol) and dioxane (140 mL) were mixed and stirred under nitrogen, and then hydrochloric acid (23.0 mL, 140 mmol) was added to the above mixture, and heated to The reaction was carried out at 85°C for 18 hours. After cooling the reaction, the solvent was removed by concentration. After dissolving the crude product in THF until it has low viscosity and fluidity, the insoluble matter is filtered off. The solution was then added to n-hexane for reprecipitation, and the filter cake was collected by filtration. After drying the filter cake, a white solid PMAA- b -P i BMA (acid value of about 280-305 mg KOH/g) was obtained. PMAA- b -P i BMA has Mw=2100, Mn=1400, and PDI=1.5. Next, 30 g of PMAA- b -P i BMA powder was stirred and dispersed in 72 mL of deionized water, and a 28% ammonia solution (11 g) was added dropwise to the above dispersion, and then heated to 70 °C for 5 hours. After completely dissolving, the pH value of the above solution was adjusted to above 8 with ammonia water to obtain double-block copolymer DBDI-02 (solid content: 26.8 wt%). The above reaction is as follows:

Synthesis Example 3 (DBDT-01) After PMDETA (12.18 g, 70.32 mmole) was dissolved in THF (65 mL), nitrogen was passed through the THF solution to deoxygenate. Then CuBr (10.08 g, 70.32 mmole) was added to the solution and stirred well. Then CuBr ₂ (3.14 g, 14.06 mmole) was added to the THF solution and stirred well.

tBMA (100 g, 703.23 mmole), p -TsCl (13.40 g, 70.32 mmole) were dissolved in THF (65 mL) and nitrogen was bubbled through the THF solution to deoxygenate. After this solution was added to the PMDETA solution, the above reactants were heated to 40°C under nitrogen for 22 hours to form PtBMA . The above-mentioned polymerization mechanism is ATRP, and its reaction formula is shown in the following formula:

Nitrogen gas was introduced into tetrahydrofuran methacrylate (THFMA, 119.70 g, 703.23 mmole) to deoxygenate, then the deoxygenated THFMA was added to the PtBMA solution, and the above reaction was heated to 40 °C under nitrogen for 24 hours to form The bi-block copolymer PtBMA - b -PTHFMA. It can be understood that since the two monomer systems of tBMA and THFMA react sequentially rather than simultaneously, the resulting copolymer is a biblock copolymer rather than a random copolymer. The above-mentioned polymerization mechanism is ATRP, and its reaction is as follows:

After the above reaction was cooled, the crude product solution after the above reaction was filtered with a neutral alumina column, and the filtrate was reprecipitated with n-hexane, and a white solid (P t BMA- b -PTHFMA) was collected. The above product had a Mw of 3600, a Mn of 2400, and a PDI of 1.5. In the above formula, m=9, n=5.

Next, PtBMA - b -PTHFMA (151 g, 64.01 mmol) and dioxane (300 mL) were mixed and stirred under nitrogen, and then hydrochloric acid (27.5 mL, 320 mmol) was added to the above mixture and heated to 85°C The reaction was carried out for 18 hours. After cooling the reaction, the solvent was removed by concentration. After dissolving the crude product in THF until it has low viscosity and fluidity, the insoluble matter is filtered off. The solution was then added to n-hexane for reprecipitation, and the filter cake was collected by filtration. After drying the filter cake, a white solid PMAA- b -PTHFMA (acid value of 210-215 mg KOH/g) was obtained. PMAA- b -PTHFMA has Mw=2700, Mn=1800, and PDI=1.5. Next, 60 g of PMAA- b -PTHFMA powder was stirred and dispersed in 60 mL of deionized water, and a 28% ammonia solution (15.2 g) was added dropwise to the above dispersion, and then heated to 70 °C to react for 5 hours. After completely dissolving, the pH value of the above solution was adjusted to above 8 with ammonia water to obtain double-block copolymer DBDT-01 (solid content: 45 wt%). The above reaction is as follows:

Synthesis Example 4 (DBMA-01) After PMDETA (12.18 g, 70.32 mmole) was dissolved in THF (65 mL), nitrogen gas was passed through the THF solution to deoxygenate. Then CuBr (10.08 g, 70.32 mmole) was added to the solution and stirred well. Then CuBr ₂ (3.14 g, 14.06 mmole) was added to the THF solution and stirred well.

After the double-necked flask was evacuated and purged with nitrogen, tBMA (100 g, 703.23 mmole), p -TsCl (13.40 g, 70.32 mmole), and THF (85 mL) were added, and nitrogen was purged into the THF solution to deoxygenate. Then, after adding this solution to the PMDETA solution, the above reactants were heated to 40°C under nitrogen for 7 hours to form PtBMA . The above-mentioned polymerization mechanism is ATRP, and its reaction formula is shown in the following formula:

Nitrogen was introduced into hydroxyethyl methacrylate (HEMA, 113.22 g, 843.88 mmole) to deoxygenate, then deoxygenated THFMA was added to the PtBMA solution, and the above reaction was heated to 40 °C under nitrogen to react for 18 hours, the bi-block copolymer PtBMA - b -PHEMA was formed. It can be understood that since the two monomer systems of tBMA and HEMA react sequentially rather than simultaneously, the resulting copolymer is a biblock copolymer rather than a random copolymer. The above-mentioned polymerization mechanism is ATRP, and its reaction is as follows:

After the above reaction was cooled, the crude product solution after the above reaction was filtered with a neutral alumina column, and the filtrate was reprecipitated with n-hexane, and a white solid (P t BMA- b -PHEMA) was collected. The above product had a Mw of 4100, a Mn of 2800, and a PDI of 1.5. In the above formula, m=11, n=7.

Next, PtBMA - b -PHEMA (120 g, 42.86 mmol) and dioxane (250 mL) were mixed and stirred under nitrogen, and then hydrochloric acid (17.9 mL, 214 mmol) was added to the above mixture and heated to 85 °C The reaction was carried out for 18 hours. After cooling the reaction, the solvent was removed by concentration. After dissolving the crude product in THF until it has low viscosity and fluidity, the insoluble matter is filtered off. The solution was then added to n-hexane for reprecipitation, and the filter cake was collected by filtration. After drying the filter cake, a white solid PMAA- b -PHEMA (acid value of 230-250 mg KOH/g) was obtained. Mw=3500, Mn=2300, and PDI=1.5 of PMAA- b -PHEMA. Next, 60 g of PMAA- b -PHEMA powder was stirred and dispersed in 93 mL of deionized water, and a 28% ammonia solution (17.1 g) was added dropwise to the above dispersion, and then heated to 70 °C for 5 hours. After the complete dissolution, the pH value of the above solution was adjusted to above 8 with ammonia water to obtain the double-block copolymer DBMA-01 (solid content: 35.5 wt%). The above reaction is as follows:

Example 1 Take 1.68 g of double-block copolymer DBDI-02 as a dispersant, add 15.32 g of water and stir to dissolve, add 3 g of carbon black (XC72R, purchased from Cabot), and continue to stir to obtain carbon black Dispersion WB38 had an average particle diameter (D _ave ) of carbon black of 305 nm and D ₉₅ of 689 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion WB38 was 0.15, and the fluidity was good.

After mixing 1.38 g of polyurethane resin (2026C, purchased from Liuhe Chemical Co., Ltd.) with 4.61 g of carbon black dispersion WB38, a conductive ink was obtained by stirring, and the average particle size (D _ave ) of the carbon black was 307 nm (ΔD _ave = 2 nm), and _D95 was 694 nm. The conductive ink was coated on the PET film with a wire bar of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. The sheet resistance (31 Ω/□/mil) of the conductive layer was measured with a four-point probe conductivity meter (5601Y, available from Quatek Co., Ltd.), and with a high-precision thickness meter (sylvac D50S display, manufacturer sylvac ) to measure the thickness of the conductive layer and estimate the volume resistance (78 mΩ·cm) of the conductive layer.

Example 2 Take 1.00 g of double-block copolymer DBDT-01 as a dispersant, add 24.50 g of water and stir to dissolve, add 4.5 g of carbon black (XC72R), and continue to stir to obtain carbon black dispersion WB24 , the average particle size (D _ave ) of the carbon black is 333 nm, and the D ₉₅ is 918 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion WB24 was 0.10, and the fluidity was good.

After mixing 2.30 g of resin (2026C) with 7.68 g of carbon black dispersion WB24, and stirring to obtain conductive ink, the average particle size (D _ave ) of the carbon black is 310 nm (ΔD _ave =-23 nm), and D ₉₅ is 718 nm. The conductive ink was coated on the PET film with a wire rod of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. Use a four-point probe conductivity meter (5601Y) to measure the sheet resistance of the conductive layer (34 Ω/□/mil), and use a high-precision thickness meter (sylvac D50S) to measure the thickness of the conductive layer and estimate the volume resistance of the conductive layer (86 mΩ·cm).

Example 3 Take 1.50 g of double-block copolymer DBDT-01 as a dispersant, add 24.00 g of water and stir to dissolve, add 4.5 g of carbon black (XC72R), and continue to stir to obtain carbon black dispersion WB25 , the average particle size (D _ave ) of the carbon black is 315 nm, and the D ₉₅ is 757 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion WB25 was 0.15, and the fluidity was good.

After mixing 2.30 g of resin (2026C) with 7.68 g of carbon black dispersion WB25, and stirring to obtain a conductive ink, the average particle size (D _ave ) of the carbon black is 329 nm (ΔD _ave =14 nm), and D ₉₅ is 933 nm. The conductive ink was coated on the PET film with a wire rod of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. Use a four-point probe conductivity meter (5601Y) to measure the sheet resistance of the conductive layer (39 Ω/□/mil), and use a high-precision thickness meter (sylvac D50S) to measure the thickness of the conductive layer and estimate the volume resistance of the conductive layer (99 mΩ·cm).

Example 4 Take 1.99 g of double-block copolymer DBDT-01 as a dispersant, add 23.51 g of water and stir to dissolve, add 4.5 g of carbon black (XC72R), and continue to stir to obtain carbon black dispersion WB26 , the average particle size (D _ave ) of its carbon black is 317 nm, and D ₉₅ is 861 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion WB26 was 0.20, and the fluidity was good.

After mixing 2.30 g of resin (2026C) with 7.68 g of carbon black dispersion WB26, and stirring to obtain conductive ink, the average particle size of carbon black (D _ave ) is 313 nm (ΔD _ave =-4 nm), D ₉₅ is 595 nm. The conductive ink was coated on the PET film with a wire rod of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. Use a four-point probe conductivity meter (5601Y) to measure the sheet resistance of the conductive layer (86 Ω/□/mil), and use a high-precision thickness meter (sylvac D50S) to measure the thickness of the conductive layer and estimate the volume resistance of the conductive layer (218 mΩ·cm).

Example 5 Take 0.85 g of double-block copolymer DBMA-01 as a dispersant, add 16.15 g of water and stir to dissolve, add 3 g of carbon black (XC72R), and continue to stir to obtain carbon black dispersion WB39 , the average particle size (D _ave ) of the carbon black is 330 nm, and the D ₉₅ is 814 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion liquid WB39 was 0.10, and the fluidity was good.

After mixing 1.38 g of resin (2026C) with 4.61 g of carbon black dispersion WB39, and stirring to obtain conductive ink, the average particle size (D _ave ) of the carbon black is 536 nm (ΔD _ave =206 nm), and D ₉₅ is 1260 nm. The conductive ink was coated on the PET film with a wire rod of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. Use a four-point probe conductivity meter (5601Y) to measure the sheet resistance of the conductive layer (55 Ω/□/mil), and use a high-precision thickness meter (sylvac D50S) to measure the thickness of the conductive layer and estimate the volume resistance of the conductive layer (139 mΩ·cm).

Comparative Example 1 1.65 g of double-block copolymer DBDI-01 was taken as a dispersant, 15.35 g of water was added and dissolved with stirring, and 3 g of carbon black (XC72R) was added and continuously stirred to obtain a mixture WB44. The weight ratio (D/P) of the dispersant to carbon black in the mixture WB44 was 0.10, but it could not be dispersed and showed a colloidal state.

Comparative Example 2 Take 1.69 g of commercially available dispersant BYK2015 (solid content of 40 wt%, purchased from BYK), add 23.81 g of water and stir to dissolve, add 4.5 g of carbon black (XC72R), and continue to stir to obtain a mixture WB27. The weight ratio (D/P) of the dispersant to carbon black in the mixture WB27 was 0.15, and it was not dispersed and showed a colloidal state.

Comparative Example 3 Take 2.25 g of commercially available dispersant BYK2015, add 23.25 g of water and stir to dissolve, add 4.5 g of carbon black (XC72R), and continue to stir to obtain carbon black dispersion WB28, the average particle size of carbon black. The diameter (D _ave ) was 406 nm, and the D ₉₅ was 1180 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion liquid WB28 was 0.20, and the fluidity was poor.

After mixing 2.30 g of resin (2026C) with 7.68 g of carbon black dispersion WB28, and stirring to obtain conductive ink, the average particle size (D _ave ) of the carbon black is 346 nm (ΔD _ave =-60 nm), D ₉₅ is 1290 nm. The conductive ink was coated on the PET film with a wire rod of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. Use a four-point probe conductivity meter (5601Y) to measure the sheet resistance of the conductive layer (143 Ω/□/mil), and use a high-precision thickness meter (sylvac D50S) to measure the thickness of the conductive layer and calculate the volume resistance of the conductive layer (363 mΩ·cm).

Comparative Example 4 Take 4.50 g of commercially available dispersant BYK2015, add 21.00 g of water and stir to dissolve, add 4.5 g of carbon black (XC72R), and continue to stir to obtain carbon black dispersion WB29. The diameter (D _ave ) was 330 nm, and the D ₉₅ was 725 nm. The weight ratio (D/P) of the dispersant to carbon black in the carbon black dispersion WB29 was 0.40, and the fluidity was good.

After mixing 2.30 g of resin (2026C) with 7.68 g of carbon black dispersion WB29, and stirring to obtain conductive ink, the average particle size of carbon black (D _ave ) is 319 nm (ΔD _ave =-11 nm), D ₉₅ is 766 nm. The conductive ink was coated on the PET film with a wire rod of No. 44, heated to 150° C. and baked for 30 minutes to obtain a conductive layer. Use a four-point probe conductivity meter (5601Y) to measure the sheet resistance of the conductive layer (126 Ω/□/mil), and use a high-precision thickness meter (sylvac D50S) to measure the thickness of the conductive layer and calculate the volume resistance of the conductive layer (320 mΩ·cm).

From the comparison of Examples 1 to 5 and Comparative Examples 1 to 4, it can be seen that the amount of dispersant in the examples is small (D/P=0.10~0.15), that is, it has good dispersibility (D _ave = 305~333 nm). In addition, the conductivity of the conductive layer of the embodiment is greatly improved, and the sheet resistance is greatly reduced.

Example 6 Take 2.50 g of double-block copolymer DBDT-01 as a dispersant, add 23.00 g of water and stir to dissolve, add 4.5 g of carbon black (EMPEROR ^® 2000, purchased from Cabot), and stir for another 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K151a. The average particle size of carbon black was The diameter (D _ave ) was 76 nm and the D ₁₀₀ was 396 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K151a was 0.25, and the carbon black content was 15 wt%.

After 3.0 g of carbon black dispersion K151a was placed in an oven at 60 °C for 7 days, the average particle size (D _ave ) of the carbon black was 74 nm (ΔD _ave =-2 nm), and the D ₁₀₀ was 295 nm. After taking 3.0 g of carbon black dispersion K151a and 0.53 g of 1,2-propanediol (as an antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 71 nm. (ΔD _ave = -5 nm), D ₁₀₀ was 295 nm.

Example 7 Take 3.33 g of double-block copolymer DBDT-01 as a dispersant, add 20.67 g of water and stir to dissolve, add 6.0 g of carbon black (EMPEROR ^® 2000), and stir for another 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After the shaking was completed, it was filtered with a filter cloth with a pore size of 25 μm to obtain a carbon black dispersion K152a. The average particle size of the carbon black was The diameter (D _ave ) was 91 nm, and the D ₁₀₀ was 396 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K152a was 0.25, and the carbon black content was 20 wt%.

After 3.0 g of carbon black dispersion K152a was placed in an oven at 60 °C for 7 days, the average particle size (D _ave ) of the carbon black was 98 nm (ΔD _ave =7 nm), and the D ₁₀₀ was 396 nm. After taking 3.0 g of carbon black dispersion K152a and 0.53 g of 1,2-propanediol (as an antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 96 nm. (ΔD _ave =5 nm), D ₁₀₀ was 396 nm.

Example 8 Take 3.36 g of double block copolymer DBDI-02 as a dispersant, add 22.14 g of water and stir to dissolve, then add 4.5 g of carbon black (EMPEROR ^® 2000) and stir for 0.5 hour. After the magnet was taken out, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K153a. The average particle size of carbon black was The diameter (D _ave ) was 80 nm and the D ₁₀₀ was 342 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K153a was 0.20, and the carbon black content was 15 wt%.

After 3.0 g of carbon black dispersion K153a was placed in an oven at 60 °C for 7 days, the average particle size (D _ave ) of the carbon black was 84 nm (ΔD _ave =4 nm), and the D ₁₀₀ was 531 nm. After taking 3.0 g of carbon black dispersion K153a and 0.53 g of 1,2-propanediol (as an antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 92 nm. (ΔD _ave = 12 nm), D ₁₀₀ was 342 nm.

Example 9 Take 5.71 g of double block copolymer DBDI-02 as a dispersant, add 18.29 g of water and stir to dissolve, then add 6.0 g of carbon black (EMPEROR ^® 2000) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K154a. The average particle size of carbon black was The diameter (D _ave ) was 102 nm, and the D ₁₀₀ was 459 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K154a was 0.20, and the carbon black content was 20 wt%.

After 3.0 g of carbon black dispersion K154a was placed in an oven at 60 °C for 7 days, the average particle size (D _ave ) of the carbon black was 102 nm (ΔD _ave =0 nm), and D ₁₀₀ was 459 nm. After taking 3.0 g of carbon black dispersion K154a and 0.53 g of 1,2-propanediol (as antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 106 nm (ΔD _ave = 4 nm), D ₁₀₀ was 615 nm.

Example 10 Take 2.52 g of double block copolymer DBDI-02 as a dispersant, add 22.98 g of water and stir to dissolve, then add 4.5 g of carbon black (EMPEROR ^® 2000) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K147a. The average particle size of carbon black was The diameter (D _ave ) was 76 nm and the D ₁₀₀ was 255 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K147a was 0.15, and the carbon black content was 15 wt%.

After 3.0 g of carbon black dispersion K147a was placed in an oven at 60 °C for 7 days, the average particle size (D _ave ) of the carbon black was 89 nm (ΔD _ave =13 nm), and the D ₁₀₀ was 396 nm. After taking 3.0 g of carbon black dispersion K147a and 0.53 g of 1,2-propanediol (as an antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 111 nm. (ΔD _ave = 35 nm), D ₁₀₀ was 531 nm.

Comparative Example 5 After taking 6.75 g of commercially available dispersant BYK2015, adding 18.75 g of water and stirring to dissolve, 4.5 g of carbon black (EMPEROR ^® 2000) was added and stirred for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K179a. The average particle size of carbon black was The diameter (D _ave ) was 63 nm, and the D ₁₀₀ was 295 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K179a was 0.60, and the carbon black content was 15 wt %. It is worth noting that if the weight ratio (D/P) of dispersant to carbon black in this carbon black dispersion is reduced to 0.4 or lower, it will gel (Gel) and cannot flow.

Take 3.0 g of the carbon black dispersion K179a and put it in an oven at 60°C for 7 days and then gel and cannot flow. After taking 3.0 g of carbon black dispersion K179a and 0.53 g of 1,2-propanediol (as antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 77 nm. (ΔD _ave = 14 nm), D ₁₀₀ was 6440 nm.

Comparative Example 6 Take 7.88 g of commercially available dispersant BYK2012 (purchased from BYK), add 17.63 g of water and stir to dissolve, then add 4.5 g of carbon black (EMPEROR ^® 2000) and stir for 0.5 hour. After the magnet was taken out, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K184a. The average particle size of carbon black was The diameter (D _ave ) was 134 nm, and the D ₁₀₀ was 615 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K184a was 0.70, and the carbon black content was 15 wt %. It is worth noting that if the weight ratio (D/P) of dispersant to carbon black in this carbon black dispersion is reduced to 0.5 or less, it will gel (Gel) and cannot flow.

Take 3.0 g of the carbon black dispersion K184a and put it in an oven at 60°C for 7 days and show gelation. 3.0 g of carbon black dispersion K184a and 0.53 g of 1,2-propanediol (as an antifreeze) were put into a refrigerator at -17°C for 7 days and then gelled.

Comparative Example 7 Take 9.00 g of commercially available dispersant BYK2010 (purchased from BYK), add 16.50 g of water and stir to dissolve, then add 4.5 g of carbon black (EMPEROR ^® 2000) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K188a. The average particle size of carbon black was The diameter (D _ave ) was 105 nm, and the D ₁₀₀ was 396 nm. The weight ratio (D/P) of dispersant to carbon black in the carbon black dispersion K188a was 0.80, and the carbon black content was 15 wt %. It is worth noting that if the weight ratio (D/P) of dispersant to carbon black in this carbon black dispersion is reduced to 0.5 or less, it will gel (Gel) and cannot flow.

After taking 3.0 g of carbon black dispersion K188a and placing it in an oven at 60°C for 7 days, it was gelled and could not flow. After taking 3.0 g of carbon black dispersion K188a and 0.53 g of 1,2-propanediol (as antifreeze) and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the carbon black is 105 nm. (ΔD _ave = 0 nm), D ₁₀₀ was 615 nm.

Comparative Example 8 Take 3.65 g of commercially available dispersant BYK9151 (purchased from BYK), add 21.85 g of water and stir to dissolve, then add 4.5 g of carbon black (EMPEROR ^® 2000) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain carbon black dispersion K189a. The average particle size of carbon black was The diameter (D _ave ) was 135 nm and the D ₁₀₀ was 615 nm. The weight ratio (D/P) of the dispersant to carbon black of the carbon black dispersion K189a was 0.80, and the carbon black content was 15 wt %. It is worth noting that if the weight ratio (D/P) of dispersant to carbon black in this carbon black dispersion is reduced to 0.5 or less, it will gel (Gel) and cannot flow.

Take 3.0 g of the carbon black dispersion K189a and put it in an oven at 60°C for 7 days and show gelation. 3.0 g of carbon black dispersion K189a and 0.53 g of 1,2-propanediol (as an antifreeze) were put into a refrigerator at -17°C for 7 days and then gelled.

From the comparison of Examples 6 to 10 and Comparative Examples 5 to 8, it can be seen that the dispersants of the examples can disperse carbon black with high specific surface area up to 20 wt under the condition of less usage (D/P=0.15~0.25). %, and the stability of thermal storage and low temperature storage is good.

Example 11 Take 1.00 g of double-block copolymer DBDT-01 as a dispersant, add 14.00 g of water and stir to dissolve, add 15.00 g of titanium dioxide (TiO ₂ , CR828, purchased from the manufacturer TRONOX) and stir for 0.5 hours . After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain a titanium dioxide dispersion LAW184. The average particle size of titanium dioxide was The diameter (D _ave ) was 464 nm, the D ₉₅ was 930 nm, and the particle size distribution (D ₉₅ /D _ave ) was 2.00.

Example 12 Take 1.68 g of double-block copolymer DBDI-02 as a dispersant, add 13.32 g of water and stir to dissolve, then add 15.00 g of titanium dioxide (CR828) and stir for 0.5 hour. After taking out the magnet, add 60 g of zirconium beads (size: 0.2 mm) and shake and disperse for 8 hours. After the shaking is completed, it is filtered with a filter cloth with a filter pore size of 25 μm to obtain a titanium dioxide dispersion LAW206. The average particle size of titanium dioxide is The diameter (D _ave ) was 278 nm, the D ₉₅ was 524 nm, and the particle size distribution (D ₉₅ /D _ave ) was 1.88.

Comparative Example 9 After taking 1.13 g of commercially available dispersant BYK2015, adding 13.88 g of water and stirring to dissolve, 15.00 g of titanium dioxide (CR828) was added and stirred for 0.5 hours. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a filter pore size of 25 μm to obtain a titanium dioxide dispersion LAW211. The average particle size of titanium dioxide was The diameter (D _ave ) was 883 nm, the D ₉₅ was 4710 nm, and the particle size distribution (D ₉₅ /D _ave ) was 5.33.

From the comparison between Examples 11 and 12 and Comparative Example 9, it can be seen that using the dispersing agent of the Example to disperse the titanium dioxide, the obtained dispersion liquid has a small particle size and a narrow distribution of the titanium dioxide, showing a better dispersion effect.

Example 13 Take 2.50 g of double-block copolymer DBDT-01 as a dispersant, add 17.00 g of water and 3.00 g of 1,2-propanediol to dissolve under stirring, and add 7.50 g of blue pigment (B-432, purchased from from Fuda Pigment) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain blue dispersion B07. The particle size (D _ave ) was 122 nm and the D ₁₀₀ was 396 nm. The weight ratio (D/P) of dispersant to blue pigment of blue dispersion liquid B07 was 0.15, and the content of blue pigment was 25 wt%.

After 3.0 g of blue dispersion B07 was placed in an oven at 60°C for 7 days, the average particle size (D _ave ) of the blue pigment was 117 nm (ΔD _ave =-5 nm), and D ₁₀₀ was 396 nm. After taking 3.0 g of blue dispersion B07 and placing it in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of its blue pigment is 120 nm (ΔD _ave =-2 nm), and D ₁₀₀ is 342 nm .

Example 14 Take 4.20 g of double-block copolymer DBDI-02 as a dispersant, add 15.30 g of water and 3.00 g of 1,2-propanediol and stir to dissolve, then add 7.50 g of blue pigment (B-432) and stir 0.5 hours. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain blue dispersion B08. The particle size (D _ave ) was 118 nm and the D ₁₀₀ was 459 nm. The weight ratio (D/P) of dispersant to blue pigment of blue dispersion liquid B08 was 0.15, and the content of blue pigment was 25 wt%.

After 3.0 g of blue dispersion B08 was placed in an oven at 60°C for 7 days, the average particle size (D _ave ) of its blue pigment was 126 nm (ΔD _ave =8 nm), and D ₁₀₀ was 531 nm. After 3.0 g of blue dispersion B08 was placed in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of its blue pigment was 122 nm (ΔD _ave =4 nm), and D ₁₀₀ was 531 nm.

Example 15 Take 5.60 g of double-block copolymer DBDI-02 as a dispersant, add 13.90 g of water and 3.00 g of 1,2-propanediol, and stir to dissolve, then add 7.50 g of blue pigment (B-432) and stir 0.5 hours. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain blue dispersion B09. The particle size (D _ave ) was 125 nm and the D ₁₀₀ was 396 nm. The weight ratio (D/P) of the dispersant to the blue pigment of the blue dispersion liquid B09 was 0.20, and the content of the blue pigment was 25 wt%.

After 3.0 g of blue dispersion B09 was placed in an oven at 60°C for 7 days, the average particle size (D _ave ) of the blue pigment was 140 nm (ΔD _ave =15 nm) and D ₁₀₀ was 459 nm. After 3.0 g of blue dispersion B09 was placed in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of its blue pigment was 126 nm (ΔD _ave =1 nm), and D ₁₀₀ was 396 nm.

Example 16 Take 3.33 g of double-block copolymer DBDT-01 as a dispersant, add 17.67 g of water and 3.00 g of 1,2-propanediol, and stir to dissolve, then add 6.00 g of a yellow pigment (Y-310, purchased from Daifuku Pigment) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After the shaking was completed, it was filtered with a filter cloth with a filter pore size of 25 μm to obtain a yellow dispersion liquid Y08. The average particle size of the yellow pigment was (D _ave ) was 138 nm and D ₁₀₀ was 459 nm. The weight ratio (D/P) of dispersant to yellow pigment in yellow dispersion liquid Y08 was 0.25, and the content of yellow pigment was 18 wt%.

After 3.0 g of yellow dispersion Y08 was placed in an oven at 60 °C for 7 days, the average particle size (D _ave ) of its blue pigment was 134 nm (ΔD _ave =-4 nm), and D ₁₀₀ was 459 nm. After 3.0 g of yellow dispersion Y08 was placed in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the yellow pigment was 138 nm (ΔD _ave =0 nm), and D ₁₀₀ was 459 nm.

Example 17 Take 6.72 g of double-block copolymer DBDI-02 as a dispersant, add 14.28 g of water and 3.00 g of 1,2-propanediol, and stir to dissolve, add 6.00 g of yellow pigment (Y-310), and then add 6.00 g of yellow pigment (Y-310). Stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After the shaking was completed, it was filtered with a filter cloth with a filter pore size of 25 μm to obtain a yellow dispersion liquid Y10. The average particle size of the yellow pigment was (D _ave ) was 153 nm and D ₁₀₀ was 459 nm. The weight ratio (D/P) of the dispersant to the yellow pigment of the yellow dispersion liquid Y10 was 0.30, and the content of the yellow pigment was 20 wt%.

After 3.0 g of yellow dispersion Y10 was placed in an oven at 60°C for 7 days, the average particle size (D _ave ) of its blue pigment was 171 nm (ΔD _ave =18 nm), and D ₁₀₀ was 459 nm. After 3.0 g of yellow dispersion Y10 was placed in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the yellow pigment was 184 nm (ΔD _ave =31 nm), and D ₁₀₀ was 531 nm.

Example 18 Take 4.00 g of double-block copolymer DBDT-01 as a dispersant, add 17.00 g of water and 3.00 g of 1,2-propanediol for stirring to dissolve, and add 6.00 g of a red pigment (R-220, purchased from Daifuku Pigment) and stir for 0.5 hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain a red dispersion liquid R09, the average particle size of the red pigment. (D _ave ) was 130 nm and D ₁₀₀ was 459 nm. The weight ratio (D/P) of the dispersant to the red pigment in the red dispersion liquid R09 was 0.30, and the content of the red pigment was 20 wt%.

After 3.0 g of the red dispersion R09 was placed in an oven at 60°C for 7 days, the average particle size (D _ave ) of the blue pigment was 126 nm (ΔD _ave =-4 nm), and the D ₁₀₀ was 459 nm. After 3.0 g of the red dispersion R09 was placed in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the red pigment was 130 nm (ΔD _ave =0 nm), and the D ₁₀₀ was 459 nm.

Example 19 Take 5.60 g of double-block copolymer DBDI-02 as a dispersant, add 15.40 g of water and 3.00 g of 1,2-propanediol and stir to dissolve, then add 6.00 g of red pigment (R-220) and stir for 0.5 Hour. After taking out the magnet, 60 g of zirconium beads (size: 0.2 mm) were added and shaken and dispersed for 8 hours. After shaking, it was filtered with a filter cloth with a pore size of 25 μm to obtain a red dispersion liquid R10, the average particle size of the red pigment. (D _ave ) was 132 nm and D ₁₀₀ was 459 nm. The weight ratio (D/P) of the dispersant to the red pigment of the red dispersion liquid R10 was 0.25, and the content of the red pigment was 20 wt%.

After 3.0 g of the red dispersion R10 was placed in an oven at 60°C for 7 days, the average particle size (D _ave ) of the blue pigment was 128 nm (ΔD _ave =-4 nm), and the D ₁₀₀ was 459 nm. After 3.0 g of the red dispersion R10 was placed in a refrigerator at -17°C for 7 days, the average particle size (D _ave ) of the red pigment was 132 nm (ΔD _ave =0 nm), and the D ₁₀₀ was 459 nm.

It can be seen from Examples 13 to 19 that the dispersants of the examples can be used to disperse pigments, and the obtained dispersions have good thermal and low-temperature storage stability.

Although the present disclosure has been disclosed above with several preferred embodiments, it is not intended to limit the present disclosure. Anyone with ordinary knowledge in the technical field can make any changes without departing from the spirit and scope of the present disclosure. Therefore, the scope of protection of this disclosure should be determined by the scope of the appended patent application.

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Claims (10)

A dispersion liquid, comprising: 100 parts by weight of powder; 1 to 80 parts by weight of a dispersant; and 80 to 900 parts by weight of a polar solvent; wherein the dispersant is a double-block copolymer, and its chemical structure is:

Wherein Ini and Ini' are the residues of initiators used in the polymerization reaction; each R ¹ is independently H or methyl; R ² is

,

,or

; B is an alkali metal or N(R ³ ) ₄ , and each R ³ is independently H, a C _1-4 alkyl group, or a C _1-4 alkyl alcohol; the ratio of m to n is 3: 1 to 1:2; and x is 0.7 to 1; wherein the weight average molecular weight of the dispersant is 1500 to 4500. The dispersion liquid of claim 1, wherein the powder comprises carbon material, pigment, metal, metal oxide, or a combination thereof. The dispersion liquid of claim 2, wherein the carbon material comprises carbon black, graphite, graphene, carbon nanotubes, fullerenes, or a combination thereof. The dispersion liquid of claim 1, wherein the powder has an average particle size of 100 nm to 550 nm. The dispersion of claim 1, wherein the polar solvent comprises water, diethylene glycol diethyl ether, diethylene glycol dimethyl ether, propylene glycol methyl ether acetate, diethylene glycol butyl ether acetate, ethylene glycol butyl ether , tetraethylene glycol dimethyl ether, or a combination of the above. An ink, comprising: a dispersion liquid and a resin, and the weight ratio of the dispersion liquid to the resin is 100:10 to 100:120; wherein the dispersion liquid includes: 100 parts by weight of powder; 1 to 80 parts by weight of dispersant ; And 80 to 900 parts by weight of polar solvent; Wherein this dispersant is a double block copolymer, and its chemical structure is:

Wherein Ini and Ini' are the residues of initiators used in the polymerization reaction; each R ¹ is independently H or methyl; R ² is

,

,or

; B is an alkali metal or N(R ³ ) ₄ , and each R ³ is independently H, a C _1-4 alkyl group, or a C _1-4 alkyl alcohol; the ratio of m to n is 3: 1 to 1:2; x is 0.7 to 1; wherein the weight average molecular weight of the dispersant is 1500 to 4500. The ink of claim 6, wherein the resin comprises polypropylene resin, polyurethane resin, or a combination thereof. The ink of claim 6, wherein the powder comprises carbon material, pigment, metal, metal oxide, or a combination thereof. The ink of claim 8, wherein the carbon material comprises carbon black, graphite, graphene, carbon nanotubes, fullerenes, or a combination thereof. The ink of claim 6, wherein the powder has an average particle size of 100 nm to 550 nm.