Organic alcohol type hyperdispersant, its preparation method and high-dispersibility ABS color master batch

By preparing an organic alcohol-based superdispersant, the problem of poor dispersion performance in the three-component ABS resin system was solved, resulting in ABS masterbatch with high dispersibility and high blackness, exhibiting excellent mechanical properties.

CN116655903BActive Publication Date: 2026-03-31NINGBO COLOR MASTER BATCH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-24
Publication Date
2026-03-31

AI Technical Summary

Technical Problem

In the existing technology, the three-component system of ABS resin results in complex melt flow, non-uniform resin properties, and difficulty in meeting high requirements for the dispersion performance of color masterbatch.

Method used

Highly dispersible ABS masterbatch is prepared using an organic alcohol-based superdispersant composed of lauryl alcohol, ethylene oxide, and a catalyst in a specific ratio. The catalyst is used to adjust the acidity of the reaction and neutralize the reaction environment to ensure the stability of the reaction system.

Benefits of technology

It achieves high dispersibility and high blackness of ABS masterbatch, with a dispersibility of 75% and a blackness of 85, and also has good mechanical properties.

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Abstract

The application belongs to the technical field of color master batch materials, and relates to an organic alcohol type hyperdispersant, a preparation method thereof and ABS color master batch with high dispersibility. The application discloses an organic alcohol type hyperdispersant, components of the organic alcohol type hyperdispersant, by weight fraction, including: lauryl alcohol 30-60 parts, ethylene oxide 90-110 parts, a first catalyst 1-10 parts, a second catalyst 120-165 parts, chloropropionic acid 75-120 parts. The application also discloses a preparation method of the organic alcohol type hyperdispersant, and the preparation method comprises the following steps: S1, after heating lauryl alcohol, the first catalyst is added and mixed, ethylene oxide is added dropwise, and then a first heating reaction is carried out to obtain an intermediate; S2, after heating the intermediate, the second catalyst is added and mixed, chloropropionic acid is added dropwise, and then a second heating reaction is carried out to obtain the organic alcohol type hyperdispersant. The application also discloses ABS color master batch containing 4-8% of the organic alcohol type hyperdispersant, and the ABS color master batch has high dispersibility and high blackness.
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Description

Technical Field

[0001] This invention belongs to the field of color masterbatch technology, and relates to an organic alcohol type superdispersant, its preparation method, and highly dispersible ABS color masterbatch. Background Technology

[0002] ABS resin is a high-demand, rapidly developing polymer material that falls between engineering plastics and general-purpose plastics. It possesses excellent comprehensive physical and mechanical properties and is widely used in electronics, electrical appliances, automobiles, textiles, construction, and consumer goods. To expand its applications and ensure the coloring effect and mechanical properties of the products, specialized color masterbatches are used for coloring. ABS resin is composed of block-polymer acrylonitrile, butadiene, and styrene monomers. However, these three components are not linked together to form a single phase but rather a two-phase system. Polymers with different chemical properties exist in different phases, resulting in complex melt flow. Furthermore, different proportions of the three components lead to variations in the resin's properties, which places higher demands on the dispersion performance of the color masterbatch. Summary of the Invention

[0003] The purpose of this invention is to address the aforementioned problems in the prior art by proposing an organic alcohol-based superdispersant and a highly dispersible ABS masterbatch prepared therefrom, which has good dispersibility and high blackness.

[0004] The objective of this invention can be achieved through the following technical solutions:

[0005] An organic alcohol-based superdispersant, wherein the components of the organic alcohol-based superdispersant, by weight parts, comprise:

[0006] 30-60 parts lauryl alcohol, 90-110 parts ethylene oxide, 1-10 parts first catalyst, 120-165 parts second catalyst, and 75-120 parts chloropropionic acid.

[0007] Preferably, the first catalyst accounts for 1-3% of the total amount, and the second catalyst accounts for 30-45% of the total amount.

[0008] Further preferred, the first catalyst is acetic acid, and the second catalyst is a base.

[0009] Further preferred, the second catalyst is sodium hydroxide.

[0010] Preferably, the mass ratio of lauryl alcohol to ethylene oxide is 1:(1.8-2.2).

[0011] A method for preparing an organic alcohol-type hyperdispersant, the method comprising:

[0012] S1. After heating lauryl alcohol, the first catalyst is added and mixed, followed by the dropwise addition of ethylene oxide, and then the first heating reaction is carried out to obtain the intermediate.

[0013] S2. After heating the intermediate, add the second catalyst and mix, then add chloropropionic acid dropwise, and then carry out a second heating reaction to obtain an organic alcohol type superdispersant.

[0014] Preferably, the intermediate is lauryl alcohol polyoxyethylene ether.

[0015] Preferably, the heating temperature of lauryl alcohol in step S1 is 100-120°C; and the dropping time of ethylene oxide is 1-2 hours.

[0016] Preferably, the first heating reaction in step S1 is carried out at a temperature of 120–150°C for 3–5 hours.

[0017] As a preferred option, the mass ratio of lauryl alcohol, the first catalyst, and ethylene oxide in step S1 is (4-10):1:(11-20).

[0018] Preferably, the intermediate obtained in step S1 is neutralized with glacial acetic acid to a pH of 4.8–5.2 when cooled to 80–100°C.

[0019] Preferably, in step S2, the intermediate is heated at 50–65°C, the second heating reaction is carried out at 60–80°C, and the time is 3–5 hours.

[0020] Preferably, the chloropropionic acid is added in step S2 over a period of 1 to 2 hours.

[0021] Preferably, the mass ratio of the second catalyst to chloropropionic acid in step S2 is (1-2):(0.5-1).

[0022] A highly dispersible ABS masterbatch containing 4-8% organic alcohol-based superdispersant.

[0023] As a preferred option, the components of the highly dispersible ABS masterbatch, by weight, include: 50-80 parts of PA-765 ABS resin, 50-70 parts of PA-727 ABS resin, 50-70 parts of PA-756 ABS resin, 10-40 parts of carbon black, 10-20 parts of organic alcohol-type superdispersant, and 1-10 parts of other additives.

[0024] Further optimization yields a carbon black to organic alcohol-type superdispersant mass ratio of (1.5–3):1.

[0025] As a preferred option, highly dispersible ABS masterbatches can achieve a dispersibility of up to 75% and a blackness of up to 85.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] 1. The organic alcohol-type superdispersant of the present invention makes the reaction system acidic by adding a first catalyst, which causes a depolymerization reaction and accelerates the reaction rate. Adding a second catalyst neutralizes the acidic environment of the previous reaction, balances the pH, and keeps the reaction system stable.

[0028] 2. The organic alcohol-type superdispersant prepared by this invention has the characteristics of uniform dispersion and good stability; and is an important intermediate in the pharmaceutical, food, fragrance, dye and pesticide industries.

[0029] 3. The ABS masterbatch containing 4-8% organic alcohol-type superdispersant in this invention has high dispersibility and high blackness, with dispersibility reaching 75% and blackness reaching 85.

[0030] 4. The organic alcohol-type superdispersant of the present invention can be used in highly dispersible ABS masterbatches. There are many gaps in the masterbatch molecules. During the experimental reaction, the dispersant can penetrate into the gaps in the masterbatch molecules, reducing the surface tension of the particles. At the same time, the dispersant can also coat the surface of the masterbatch, using spatial isolation to prevent the aggregation between masterbatch molecules, thus keeping the masterbatch in a stable state. In addition, the addition of this dispersant can also increase the lubricity between particles, reduce surface tension, and improve the flowability of the masterbatch. Detailed Implementation

[0031] The following are specific embodiments of the present invention, which further describe the technical solution of the present invention, but the present invention is not limited to these embodiments.

[0032] Unless otherwise specified, the raw materials used in this invention are all commercially available products, and the methods used are all conventional technical means.

[0033] National standard for dispersion testing: GB / T21868.1-2008;

[0034] National standard for mechanical property testing: GB / T1040-1BA.

[0035] Example 1

[0036] Preparation of organic alcohol-based hyperdispersants:

[0037] 50 parts of lauryl alcohol were placed in a four-necked flask and heated to 100°C. 8 parts of the first catalyst (acetic acid) were added and mixed thoroughly. Nitrogen gas was introduced to replace the air. Then, the temperature was raised to 120°C, and 98 parts of liquid ethylene oxide were added dropwise while stirring for 2 hours. After the addition was completed, the reaction was kept at the temperature for 4 hours. After the reaction was completed, the temperature was allowed to drop naturally. When the temperature dropped to 95°C, the material was discharged into a beaker and neutralized with glacial acetic acid to a pH of 5.0 to obtain the intermediate lauryl alcohol polyoxyethylene ether.

[0038] The intermediate lauryl alcohol polyoxyethylene ether was heated to 60°C, and then 150 parts of the second catalyst (sodium hydroxide) were added and mixed evenly. Then 100 parts of chloropropionic acid were added dropwise over a period of 1.5 hours. After the addition was completed, the reaction was kept at the temperature for 3 hours. After the reaction was completed, the mixture was allowed to cool naturally to obtain a pale yellow liquid, which was an organic alcohol type superdispersant.

[0039] Preparation of highly dispersible ABS masterbatch:

[0040] Weigh the raw materials according to the proportions:

[0041] 70 parts of PA-765 ABS resin, 65 parts of PA-727 ABS resin, 60 parts of PA-756 ABS resin, 30 parts of HCS-200R carbon black, 15 parts of organic alcohol-based superdispersant, and 5 parts of other additives were mixed in a torque rheometer to obtain a highly dispersible ABS masterbatch.

[0042] The obtained highly dispersible ABS masterbatch has a balance torque of 25 N·m, a dispersibility of 72%, a tensile strength of 50 MPa, an elongation at break of 125%, and a blackness of 84.

[0043] Example 2

[0044] Preparation of organic alcohol-based hyperdispersants:

[0045] 50 parts of lauryl alcohol were placed in a four-necked flask and heated to 115°C. 7 parts of the first catalyst (acetic acid) were added and mixed thoroughly. Nitrogen gas was introduced to replace the air. Then, the temperature was raised to 120°C and 102 parts of liquid ethylene oxide were added dropwise while stirring for 2 hours. After the addition was completed, the reaction was kept at the temperature for 4 hours. After the reaction was completed, the temperature was allowed to drop naturally. When the temperature dropped to 95°C, the material was discharged into a beaker and neutralized with glacial acetic acid to a pH of 5.0 to obtain the intermediate lauryl alcohol polyoxyethylene ether.

[0046] The intermediate lauryl alcohol polyoxyethylene ether was heated to 60°C, and then 150 parts of the second catalyst (sodium hydroxide) were added and mixed evenly. Then 100 parts of chloropropionic acid were added dropwise over a period of 1.5 hours. After the addition was completed, the reaction was kept at the temperature for 3 hours. After the reaction was completed, the mixture was allowed to cool naturally to obtain a pale yellow liquid, which was an organic alcohol type superdispersant.

[0047] Preparation of highly dispersible ABS masterbatch:

[0048] Weigh the raw materials according to the proportions:

[0049] 65 parts of PA-765 ABS resin, 65 parts of PA-727 ABS resin, 65 parts of PA-756 ABS resin, 30 parts of HCS-200R carbon black, 17 parts of organic alcohol-type superdispersant, and 3 parts of other additives were placed in a torque rheometer for blending to obtain a highly dispersible ABS masterbatch.

[0050] The obtained highly dispersible ABS masterbatch has a balance torque of 22 N·m, a dispersibility of 75%, a tensile strength of 53 MPa, an elongation at break of 140%, and a blackness of 85.

[0051] Example 3

[0052] Preparation of organic alcohol-based hyperdispersants:

[0053] 50 parts of lauryl alcohol were placed in a four-necked flask and heated to 110°C. 8 parts of the first catalyst (acetic acid) were added and mixed thoroughly. Nitrogen gas was introduced to replace the air. Then, the temperature was raised to 120°C, and 100 parts of liquid ethylene oxide were added dropwise while stirring for 2 hours. After the addition was completed, the reaction was kept at the temperature for 4 hours. After the reaction was completed, the temperature was allowed to drop naturally. When the temperature dropped to 95°C, the material was discharged into a beaker and neutralized with glacial acetic acid to a pH of 5.0 to obtain the intermediate lauryl alcohol polyoxyethylene ether.

[0054] The intermediate lauryl alcohol polyoxyethylene ether was heated to 60°C, and then 55 parts of the second catalyst (sodium hydroxide) were added and mixed evenly. Then 30 parts of chloropropionic acid were added dropwise over a period of 1.5 hours. After the addition was completed, the reaction was kept at the temperature for 3 hours. After the reaction was completed, the mixture was allowed to cool naturally to obtain a pale yellow liquid, which was an organic alcohol type superdispersant.

[0055] Preparation of highly dispersible ABS masterbatch:

[0056] Weigh the raw materials according to the proportions:

[0057] 60 parts of PA-765 ABS resin, 65 parts of PA-727 ABS resin, 70 parts of PA-756 ABS resin, 30 parts of HCS-200R carbon black, 16 parts of organic alcohol-type superdispersant, and 4 parts of other additives were placed in a torque rheometer for blending to obtain a highly dispersible ABS masterbatch.

[0058] The obtained highly dispersible ABS masterbatch has a balance torque of 24 N·m, a dispersibility of 70%, a tensile strength of 52 MPa, an elongation at break of 130%, and a blackness of 83.

[0059] Example 4

[0060] Compared with Example 1, the difference lies in the fact that in the preparation of the highly dispersible ABS masterbatch, the raw materials include the following components: 70 parts of PA-765 type ABS resin, 65 parts of PA-727 type ABS resin, 60 parts of PA-756 type ABS resin, 30 parts of HCS-200R type carbon black, 10 parts of organic alcohol type superdispersant, and 10 parts of other additives.

[0061] The obtained highly dispersible ABS masterbatch has a balance torque of 21 N·m, a dispersibility of 68%, a tensile strength of 49 MPa, an elongation at break of 115%, and a blackness of 80.

[0062] Example 5

[0063] Compared with Example 1, the difference lies in the preparation of the highly dispersible ABS masterbatch, in which the raw materials include the following components: 65 parts of PA-765 type ABS resin, 60 parts of PA-727 type ABS resin, 60 parts of PA-756 type ABS resin, 30 parts of HCS-200R type carbon black, 25 parts of organic alcohol type superdispersant, and 5 parts of other additives.

[0064] The obtained highly dispersible ABS masterbatch has a balance torque of 19 N·m, a dispersibility of 70%, a tensile strength of 40 MPa, an elongation at break of 102%, and a blackness of 88.

[0065] In this embodiment, an excessive amount of organic alcohol-type superdispersant was added, resulting in an excessive amount of superdispersant covering the surface of the masterbatch particles, which affected the transfer of mechanical energy and reduced shear force.

[0066] Example 6

[0067] Compared with Example 1, the difference lies in the fact that in the preparation of the highly dispersible ABS masterbatch, the raw materials include the following components: 195 parts of PA-765 type ABS resin, 30 parts of HCS-200R type carbon black, 15 parts of organic alcohol type superdispersant, and 5 parts of other additives.

[0068] The obtained highly dispersible ABS masterbatch has a balance torque of 23 N·m, a dispersibility of 67%, a tensile strength of 51 MPa, an elongation at break of 127%, and a blackness of 77.

[0069] Example 7

[0070] Compared with Example 1, the difference lies in the preparation process of the organic alcohol-type superdispersant, which includes:

[0071] 40 parts of lauryl alcohol were placed in a four-necked flask and heated to 100°C. 15 parts of the first catalyst (acetic acid) were added and mixed thoroughly. Nitrogen gas was introduced to replace the air. Then, the temperature was raised to 120°C and 103 parts of liquid ethylene oxide were added dropwise while stirring for 2 hours. After the addition was completed, the reaction was kept at the temperature for 4 hours. After the reaction was completed, the temperature was allowed to drop naturally. When the temperature dropped to 95°C, the material was discharged into a beaker and neutralized with glacial acetic acid to a pH of 5.0 to obtain the intermediate lauryl alcohol polyoxyethylene ether.

[0072] The intermediate lauryl alcohol polyoxyethylene ether was heated to 60°C, and then 150 parts of the second catalyst (sodium hydroxide) were added and mixed evenly. Then 100 parts of chloropropionic acid were added dropwise over a period of 1.5 hours. After the addition was completed, the reaction was kept at the temperature for 3 hours. After the reaction was completed, the mixture was allowed to cool naturally to obtain a pale yellow liquid, which was an organic alcohol type superdispersant.

[0073] The obtained highly dispersible ABS masterbatch has a dispersibility of 65% and a blackness of 74.

[0074] In this embodiment, an excess of the first catalyst was added during the preparation of the organic alcohol-type superdispersant, which led to an accelerated reaction rate and a rapid increase in temperature in a short period of time. This may result in the generation of other by-products, and will also affect the dispersion performance of the superdispersant, as well as cause waste.

[0075] Example 8

[0076] The difference compared to Example 1 lies in the preparation process of the organic alcohol-type hyperdispersant:

[0077] The intermediate lauryl alcohol polyoxyethylene ether was heated to 60°C, and then 115 parts of the second catalyst (sodium hydroxide) were added and mixed evenly. Then 135 parts of chloropropionic acid were added dropwise over a period of 1.5 hours. After the addition was completed, the reaction was kept at the temperature for 3 hours. After the reaction was completed, the mixture was allowed to cool naturally to obtain a pale yellow liquid, which was an organic alcohol type superdispersant.

[0078] The obtained highly dispersible ABS masterbatch has a dispersibility of 60% and a blackness of 71.

[0079] In this embodiment, the amount of the second catalyst added during the preparation of the organic alcohol-type superdispersant was too small, which led to a decrease in the reaction rate and may have resulted in the raw materials not reacting completely, thus reducing the yield.

[0080] Comparative Example 1

[0081] Using AC-6A type ABS dispersant produced by Guangzhou Yinuo Chemical Co., Ltd., and following the method described in Example 1, 70 parts of PA-765 type ABS resin, 65 parts of PA-727 type ABS resin, 60 parts of PA-756 type ABS resin, 30 parts of HCS-200R type carbon black, 15 parts of AC-6A type ABS dispersant, and 5 parts of other additives were placed in a torque rheometer for blending to obtain ABS masterbatch.

[0082] The prepared ABS masterbatch has a balance torque of 27 N·m, a dispersibility of 60%, a tensile strength of 45 MPa, an elongation at break of 102%, and a blackness of 75.

[0083] Comparative Example 2

[0084] The difference from Example 1 is that no organic alcohol-type superdispersant is added.

[0085] According to the method described in Example 1: 70 parts of PA-765 ABS resin, 65 parts of PA-727 ABS resin, 60 parts of PA-756 ABS resin, 30 parts of HCS-200R carbon black, and 5 parts of other additives were placed in a torque rheometer for blending to obtain ABS masterbatch.

[0086] The prepared ABS masterbatch has a balance torque of 29 N·m, a dispersibility of 50%, a tensile strength of 40 MPa, an elongation at break of 90%, and a blackness of 71.

[0087] In summary, the ABS masterbatch containing 4-8% organic alcohol-type superdispersant of the present invention has high dispersibility and high blackness, and the raw material ratio makes the ABS masterbatch have good mechanical properties.

[0088] The specific embodiments described herein are merely illustrative of the spirit of the invention. Those skilled in the art to which this invention pertains may make various modifications or additions to the described specific embodiments or use similar methods to substitute them, without departing from the spirit of the invention or exceeding the scope defined by the appended claims.

Claims

1. A high dispersibility ABS color masterbatch, characterized in that, The high-dispersible ABS color master batch comprises, by weight fraction, 50-80 parts of PA-765 type ABS resin, 50-70 parts of PA-727 type ABS resin, 50-70 parts of PA-756 type ABS resin, 10-40 parts of carbon black, 10-20 parts of organic alcohol type hyperdispersant, and 1-10 parts of other additives. The preparation method of the organic alcohol type hyperdispersant comprises: S1, heating lauryl alcohol, adding a first catalyst acetic acid, and then adding dropwise ethylene oxide, followed by first heating reaction to obtain an intermediate; The mass ratio of lauryl alcohol, the first catalyst, and ethylene oxide is (4-10):1:(11-20); the first heating reaction temperature is 120℃, and the time is 3-5h; S2, heating the intermediate, adding a second catalyst sodium hydroxide, and then adding dropwise chloropropionic acid, followed by second heating reaction to obtain the organic alcohol type hyperdispersant; The mass ratio of the second catalyst and chloropropionic acid is (1-2):(0.5-1); the second heating reaction temperature is 60-80℃, and the time is 3-5h; The dispersibility of the high-dispersible ABS color master batch reaches 75%. The first catalyst accounts for 1-3% of the organic alcohol type hyperdispersant, and the second catalyst accounts for 30-45%.

2. The highly dispersible ABS color masterbatch as claimed in claim 1, wherein, The mass ratio of lauryl alcohol and ethylene oxide is 1:(1.8-2.2).

3. The highly dispersible ABS color masterbatch as claimed in claim 1, wherein, The heating temperature of lauryl alcohol in step S1 is 100-120℃, and the dropwise adding time of ethylene oxide is 1-2h.

4. The highly dispersible ABS color masterbatch as claimed in claim 1, wherein, The heating temperature of the intermediate in step S2 is 50-65℃.

5. The highly dispersible ABS color masterbatch as claimed in claim 1, wherein, It contains 4-8% of the organic alcohol type hyperdispersant.

6. The highly dispersible ABS color masterbatch as claimed in claim 1 wherein, ​

Citation Information

Patent Citations

  • ABS color masterbatch and preparation method thereof

    CN108841132A