Preparation processes for high-durability chemical mechanical polishing polyurethane material and polishing and cleaning brush comprising same

Through the one-step polymerization of highly crystalline terminal hydroxy polybutylene adipate and plant fiber and lignin-enhanced polyurethane materials, the wear resistance and deformation problems of chemical mechanical polishing brushes are solved, and efficient deformation recovery and stability improvement are achieved.

WO2025167296A1PCT designated stage Publication Date: 2025-08-14GUANGZHOU AOQUN NEW MATERIALS CO LTD
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Patent Information

Application Number
PCT/CN2024/137021
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-02-06
Filing Date
2024-12-05
Publication Date
2025-08-14

AI Technical Summary

Technical Problem

The existing chemical mechanical polishing brushes have problems of insufficient wear resistance and high deformation rate during use, especially after long-term use, the bristles deform severely, which affects the polishing effect.

Method used

Highly crystalline end-hydroxy polybutylene adipate is used as the soft segment, and polyurethane material is prepared through one-step polymerization, combining the addition of plant fibers and lignin to enhance the use of fillers, improve the toughness and deformation recovery ability of the material. At the same time, a reinforced polyurethane material is installed on the non-woven fabric to provide a good support framework.

Benefits of technology

It effectively improves the material's wear resistance and deformation resistance, ensures the stability and deformation recovery efficiency of polishing brushes, and extends service life.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present disclosure relates to the technical field of polyurethane material processing. Provided are preparation processes for a high-durability chemical mechanical polishing polyurethane material and a polishing and cleaning brush comprising same. The chemical mechanical polishing polyurethane material is prepared by using a non-woven fabric as a base material and arranging a reinforced polyurethane material on the non-woven fabric, wherein the reinforced polyurethane material is obtained by preparing polyurethane from poly(1,4-butylene adipate) diol, dibutyltin dilaurate, bis(4-hydroxyphenyl)disulfide and isophorone diisocyanate, and then mixing same with pretreated plant fibers, modified lignin, a reinforcing filler, castor oil and stannous octoate. The present disclosure overcomes defects in the prior art, efficiently improves the wear resistance and fracture resistance of the material while effectively preventing the deformation thereof, and also improves the deformation recovery ratio, thereby effectively ensuring the effectiveness and stability of the polyurethane material for use as a chemical mechanical polishing brush.
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Description

A highly durable chemical mechanical polishing polyurethane material and a preparation process for its polishing cleaning brush Technical Field

[0001] The present disclosure relates to the technical field of polyurethane material processing, and in particular to a highly durable chemical mechanical polishing polyurethane material and a preparation process of a polishing cleaning brush thereof. Background Art

[0002] Chemical mechanical polishing is a technology that combines chemical and mechanical actions. The process generally involves first allowing the workpiece surface material to react chemically with the oxidant, catalyst, etc. in the polishing liquid to form a soft layer that is relatively easy to remove. The soft layer is then removed under the mechanical action of the abrasive and polishing pad in the polishing liquid, exposing the workpiece surface again. The chemical reaction is then carried out again, thus completing the workpiece surface polishing through the alternating chemical and mechanical processes. Technical issues

[0003] Polishing pads used in chemical mechanical polishing are generally made of polyurethane. While ensuring a good polishing effect, the material itself must also have good wear resistance. With the overall improvement of the overall technology of the industrial system and the development of high-precision machinery, the surface quality requirements of parts are constantly increasing. The development of precision and ultra-precision machining has also posed new challenges to the grinding and polishing performance and durability of traditional grinding tools. However, polishing pads can generally only grind flat surfaces and cannot effectively grind curved surfaces and corner sections. In this case, using a brush for grinding is a good measure. Patent No. CN 110528287 A discloses a brush-type high-durability chemical mechanical polishing polyurethane material and its preparation method. The method achieves good polishing and grinding effects by compounding polyurethane material and filler onto non-woven fabric to prepare a brush. However, in addition to wear during use, the polyurethane brush also has a certain deformation rate. In particular, after long-term use, some bristles will deform, which will seriously reduce the polishing effect. Therefore, while ensuring that the material has good wear resistance and breakage resistance, it must also have good deformation resistance. Technical Solutions

[0004] In response to the shortcomings of the existing technology, the present disclosure provides a highly durable chemical mechanical polishing polyurethane material and a polishing cleaning brush preparation process thereof, which effectively improves the wear resistance and anti-bending effect of the material while effectively preventing the deformation of the material and improving the deformation recovery efficiency, thereby effectively ensuring the effectiveness and stability of the polyurethane material when used as a chemical mechanical polishing brush.

[0005] To achieve the above objectives, the technical solution of the present disclosure is implemented through the following technical solutions:

[0006] A preparation process of a highly durable chemical mechanical polishing polyurethane material, wherein the polyurethane material is obtained by drying reinforced polyurethane material on both sides of a non-woven fabric, and the specific preparation process comprises the following steps:

[0007] (1) Plant fiber pretreatment: Select plant fibers, dry them, cut them into short pieces, then modify them with acid or alkali, and dry them again to obtain pretreated plant fibers for use;

[0008] (2) Lignin pretreatment: lignin is steam-exploded and then dried to obtain modified lignin for later use;

[0009] (3) Preparation of polyurethane: poly(1,4-butylene adipate) diol, dibutyltin dilaurate and bis(4-hydroxyphenyl) disulfide are dried and mixed, and solvent A is added and heated to dissolve to obtain a mixed solution, and isophorone diisocyanate is then added dropwise to carry out polymerization reaction, and solvent A is removed and dried to obtain polyurethane for use;

[0010] (4) Mixing: The reinforcing filler, modified lignin and pretreated plant fiber are mixed and added to solvent B, castor oil is added and ultrasonically homogenized, and then the polyurethane and stannous octoate are added and stirred thoroughly to obtain a mixed slurry for use;

[0011] (5) Coating: Pour the mixed slurry into the mold box and cover it with non-woven fabric. Slightly shake until the mixed slurry is fully in contact with the non-woven fabric, then heat and dry. After drying, take out the non-woven fabric and pour the mixed slurry into the mold box again. Then cover the non-woven fabric with the other side facing down on the slurry. Finally, place a non-woven fabric with a weight of 100-200g / cm 2 The board is continued to dry, then washed with water, and the surface is polished smooth after drying to obtain a highly durable chemical mechanical polishing polyurethane material.

[0012] Preferably, the non-woven fabric has a thickness of 1.5-2.5 mm, and after the reinforced polyurethane material is provided on both sides of the non-woven fabric, the total thickness is 3.0-3.5 mm.

[0013] Preferably, the plant fiber in step (1) is any one of ramie fiber and coconut fiber or a combination of two thereof.

[0014] Preferably, the length of the chopped plant fibers in step (1) is 1-2 cm, and the acid-base modification method is to first soak them in a solution with a pH of 4.5-5.0 for 40-60 minutes, then adjust the pH to 9.0, heat them to 55-60°C and continue soaking for 20-40 minutes, then take them out, wash them to neutrality and then dry them.

[0015] Preferably, the lignin is exploded in step (2) by steam explosion at a pressure of 2 MPa and a temperature of 121° C. for 60-65 seconds, and then dried at a temperature of 60° C. to a constant weight.

[0016] Preferably, in step (3), the mass ratio of poly(1,4-butylene adipate) diol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide is 20:0.36:5, and isophorone diisocyanate is added in a stoichiometric ratio of NCO to OH.

[0017] Preferably, the solvent A in step (3) is a mixture of 1,4-dioxane and N,N-dimethylformamide in a mass ratio of 1:3.

[0018] Preferably, the temperature for heating and dissolving in step (3) is 60°C, the temperature for polymerization reaction is 65°C, and the polymerization reaction time is 6-8h.

[0019] Preferably, the reinforcing filler in step (4) is a mixture of nano-titanium dioxide powder, nano-calcium carbonate powder, and layered graphite in a mass ratio of 1:2:1, and the solvent B is tetrachloroethane.

[0020] Preferably, in step (4), the mass ratio of the reinforcing filler, modified lignin, pretreated plant fiber, castor oil, polyurethane, stannous octoate and solvent B is 0.2-0.4:0.1-0.2:1-1.2:0.1-0.2:7:0.05-0.08:7.

[0021] Preferably, the temperature for heating and drying in step (5) is 70-90°C.

[0022] The bristles of the cleaning brush are made of the above-mentioned highly durable chemical mechanical polishing polyurethane material, which is cut and polished to a required diameter before being installed on the brush disc. Beneficial effects

[0023] The present disclosure provides a highly durable chemical mechanical polishing polyurethane material and a process for preparing the same, which has the following advantages over the prior art:

[0024] (1) The present invention adopts highly crystalline end-hydroxy polybutylene adipate (HTPBA) as the soft segment and selects a small molecule diol with a dynamic disulfide bond as a chain extender to prepare a polyurethane material through one-step polymerization. The toughness of the material is subsequently improved by adding plant fiber and lignin. While effectively improving the material's anti-deformation ability, it can also provide it with a good deformation recovery effect, thereby preventing the subsequent prepared brush from deforming during use.

[0025] (2) The present invention effectively ensures the wear resistance and hardness of the material by adding reinforcing fillers, and adsorbs the fillers through modified plant fibers and lignin. After being compounded with non-woven fabrics, it can provide a good supporting skeleton for the polyurethane materials on both sides of the non-woven fabrics, improve the permeability and connectivity of the material, and ensure the overall stability of the material. Implementation of the present disclosure

[0026] To make the objectives, technical solutions, and advantages of the embodiments of the present disclosure more clear, the technical solutions in the embodiments of the present disclosure are clearly and completely described below in conjunction with the embodiments of the present disclosure. Obviously, the described embodiments are part of the embodiments of the present disclosure, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present disclosure without making any creative efforts shall fall within the scope of protection of the present disclosure.

[0027] The main raw materials and reagents of the following examples and comparative examples are shown in Table 1:

[0028]

[0029] The solvent A is obtained by mixing 1,4-dioxane and N,N-dimethylformamide in a mass ratio of 1:3; the reinforcing filler is obtained by mixing nano-titanium dioxide powder, nano-calcium carbonate powder and layered graphite in a mass ratio of 1:2:1.

[0030] Example 1:

[0031] Preparation of chemical mechanical polishing polyurethane materials:

[0032] (1) Select ramie fiber, dry it to a moisture content of less than 8%, and then cut it into 1-2 cm fibers. Then soak the chopped fibers in a solution with a pH of 4.5 for 50 minutes, adjust the pH to 9.0, and continue soaking in a water bath at 55°C for 30 minutes. Then take it out and rinse it repeatedly with clean water until it is neutral. Then, dry the chopped fibers at 50°C to constant weight to obtain pretreated plant fibers for use.

[0033] (2) The lignin was subjected to steam explosion treatment at 121°C under a pressure of 2 MPa for 63 seconds, and then taken out and dried at 60°C to a constant weight to obtain the modified lignin for use;

[0034] (3) In an argon atmosphere, poly(1,4-butylene adipate) glycol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide were dried and mixed in a mass ratio of 20:0.36:5. Solvent A was then added in a material-liquid ratio of 1:3. The mixture was heated to 60°C and dissolved for 2 hours to obtain a mixed solution. Isophorone diisocyanate was then added dropwise to ensure the stoichiometric ratio of NCO and OH. The temperature was adjusted to 65°C for polymerization reaction for 7 hours. The mixture was then precipitated in excess water and washed to remove solvent A. The mixture was then dried in an oven at 70°C to obtain a polyurethane for standby use.

[0035] (4) The reinforcing filler, modified lignin and pretreated plant fiber were mixed and added to tetrachloroethane, and then castor oil was added and treated under 600W ultrasound for 10 minutes. Then the polyurethane and stannous octoate were added and stirred thoroughly to obtain a mixed slurry, wherein the mass ratio of the reinforcing filler, modified lignin, pretreated plant fiber, castor oil, polyurethane, stannous octoate and tetrachloroethane was 0.3:0.1:1.1:0.2:7:0.06:7.

[0036] (5) Select nylon non-woven fabric with a thickness of 2.0 mm as the base material, pour the above mixed slurry into the mold box, the thickness of the mixed slurry in the mold box is 1.0 mm, then cover the slurry with non-woven fabric of the same size as the bottom of the mold, shake it slightly until the mixed slurry is fully in contact with the non-woven fabric, then heat it to 80 ° C and dry it for 18 hours, then take out the non-woven fabric, and continue to pour 1.5 mm of mixed slurry into the mold, then cover the other side of the non-woven fabric on the mixed slurry, and then place 150 g / cm 2 The plate was pressed, and then the temperature was adjusted to 80°C and dried for 24 hours to obtain a chemical mechanical polishing polyurethane material.

[0037] Comparative Example 1:

[0038] Preparation of chemical mechanical polishing polyurethane materials:

[0039] (1) Select ramie fiber, dry it to a moisture content of less than 8%, and then cut it into 1-2 cm fibers to obtain pretreated plant fiber for later use;

[0040] (2) The lignin was subjected to steam explosion treatment at 121°C under a pressure of 2 MPa for 63 seconds, and then taken out and dried at 60°C to a constant weight to obtain the modified lignin for use;

[0041] (3) In an argon atmosphere, poly(1,4-butylene adipate) glycol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide were dried and mixed in a mass ratio of 20:0.36:5. Solvent A was then added in a material-liquid ratio of 1:3. The mixture was heated to 60°C and dissolved for 2 hours to obtain a mixed solution. Isophorone diisocyanate was then added dropwise to ensure the stoichiometric ratio of NCO and OH. The temperature was adjusted to 65°C for polymerization reaction for 7 hours. The mixture was then precipitated in excess water and washed to remove solvent A. The mixture was then dried in an oven at 70°C to obtain a polyurethane for standby use.

[0042] (4) The reinforcing filler, modified lignin and pretreated plant fiber were mixed and added to tetrachloroethane, and then castor oil was added and treated under 600W ultrasound for 10 minutes. Then the polyurethane and stannous octoate were added and stirred thoroughly to obtain a mixed slurry, wherein the mass ratio of the reinforcing filler, modified lignin, pretreated plant fiber, castor oil, polyurethane, stannous octoate and tetrachloroethane was 0.3:0.1:1.1:0.2:7:0.06:7.

[0043] (5) Select nylon non-woven fabric with a thickness of 2.0 mm as the base material, pour the above mixed slurry into the mold box, the thickness of the mixed slurry in the mold box is 1.0 mm, then cover the slurry with non-woven fabric of the same size as the bottom of the mold, shake it slightly until the mixed slurry is fully in contact with the non-woven fabric, then heat it to 80 ° C and dry it for 18 hours, then take out the non-woven fabric, and continue to pour 1.5 mm of mixed slurry into the mold, then cover the other side of the non-woven fabric on the mixed slurry, and then place 150 g / cm 2 The plate was pressed, and then the temperature was adjusted to 80°C and dried for 24 hours to obtain a chemical mechanical polishing polyurethane material.

[0044] Comparative Example 2:

[0045] Preparation of chemical mechanical polishing polyurethane materials:

[0046] (1) Select ramie fiber, dry it to a moisture content of less than 8%, and then cut it into 1-2 cm fibers. Then soak the chopped fibers in a solution with a pH of 4.5 for 50 minutes, adjust the pH to 9.0, and continue soaking in a water bath at 55°C for 30 minutes. Then take it out and rinse it repeatedly with clean water until it is neutral. Then, dry the chopped fibers at 50°C to constant weight to obtain pretreated plant fibers for use.

[0047] (2) In an argon atmosphere, poly(1,4-butylene adipate) glycol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide were dried and mixed in a mass ratio of 20:0.36:5. Solvent A was then added in a material-liquid ratio of 1:3. The mixture was heated to 60°C and dissolved for 2 hours to obtain a mixed solution. Isophorone diisocyanate was then added dropwise to ensure the stoichiometric amount of NCO and OH. The temperature was adjusted to 65°C for polymerization reaction for 7 hours. The mixture was then precipitated in excess water and washed to remove solvent A. The mixture was then dried in an oven at 70°C to obtain a polyurethane for standby use.

[0048] (3) The reinforcing filler, lignin and pretreated plant fiber were mixed and added to tetrachloroethane, and then castor oil was added and treated under 600W ultrasound for 10 minutes. Then the polyurethane and stannous octoate were added and stirred thoroughly to obtain a mixed slurry, wherein the mass ratio of reinforcing filler, modified lignin, pretreated plant fiber, castor oil, polyurethane, stannous octoate and tetrachloroethane was 0.3:0.1:1.1:0.2:7:0.06:7.

[0049] (4) Select nylon non-woven fabric with a thickness of 2.0 mm as the base material, pour the above mixed slurry into the mold box, the thickness of the mixed slurry in the mold box is 1.0 mm, then cover the slurry with non-woven fabric of the same size as the bottom of the mold, shake it slightly until the mixed slurry is fully in contact with the non-woven fabric, then heat it to 80 ° C and dry it for 18 hours, then take out the non-woven fabric, and continue to pour 1.5 mm of mixed slurry into the mold, then cover the other side of the non-woven fabric on the mixed slurry, and then place 150g / cm 2 The plate was pressed, and then the temperature was adjusted to 80°C and dried for 24 hours to obtain a chemical mechanical polishing polyurethane material.

[0050] Comparative Example 3:

[0051] Preparation of chemical mechanical polishing polyurethane materials:

[0052] (1) Select ramie fiber, dry it to a moisture content of less than 8%, and then cut it into 1-2 cm fibers to obtain pretreated plant fiber for later use;

[0053] (2) In an argon atmosphere, poly(1,4-butylene adipate) glycol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide were dried and mixed in a mass ratio of 20:0.36:5. Solvent A was then added in a material-liquid ratio of 1:3. The mixture was heated to 60°C and dissolved for 2 hours to obtain a mixed solution. Isophorone diisocyanate was then added dropwise to ensure the stoichiometric amount of NCO and OH. The temperature was adjusted to 65°C for polymerization reaction for 7 hours. The mixture was then precipitated in excess water and washed to remove solvent A. The mixture was then dried in an oven at 70°C to obtain a polyurethane for standby use.

[0054] (3) The reinforcing filler, lignin and pretreated plant fiber were mixed and added to tetrachloroethane, and then castor oil was added and treated under 600W ultrasound for 10 minutes. Then the polyurethane and stannous octoate were added and stirred thoroughly to obtain a mixed slurry, wherein the mass ratio of reinforcing filler, modified lignin, pretreated plant fiber, castor oil, polyurethane, stannous octoate and tetrachloroethane was 0.3:0.1:1.1:0.2:7:0.06:7.

[0055] (4) Select nylon non-woven fabric with a thickness of 2.0 mm as the base material, pour the above mixed slurry into the mold box, the thickness of the mixed slurry in the mold box is 1.0 mm, then cover the slurry with non-woven fabric of the same size as the bottom of the mold, shake it slightly until the mixed slurry is fully in contact with the non-woven fabric, then heat it to 80 ° C and dry it for 18 hours, then take out the non-woven fabric, and continue to pour 1.5 mm of mixed slurry into the mold, then cover the other side of the non-woven fabric on the mixed slurry, and then place 150g / cm 2 The plate was pressed, and then the temperature was adjusted to 80°C and dried for 24 hours to obtain a chemical mechanical polishing polyurethane material.

[0056] Comparative Example 4:

[0057] Preparation of chemical mechanical polishing polyurethane materials:

[0058] (1) Select ramie fiber, dry it to a moisture content of less than 8%, and then cut it into 1-2 cm fibers. Then soak the chopped fibers in a solution with a pH of 4.5 for 50 minutes, adjust the pH to 9.0, and continue soaking in a water bath at 55°C for 30 minutes. Then take it out and rinse it repeatedly with clean water until it is neutral. Then, dry the chopped fibers at 50°C to constant weight to obtain pretreated plant fibers for use.

[0059] (2) The lignin was subjected to steam explosion treatment at 121°C under a pressure of 2 MPa for 63 seconds, and then taken out and dried at 60°C to a constant weight to obtain the modified lignin for use;

[0060] (3) In an argon atmosphere, poly(1,4-butylene adipate) glycol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide were dried and mixed in a mass ratio of 20:0.36:5. Solvent A was then added in a material-liquid ratio of 1:3. The mixture was heated to 60°C and dissolved for 2 hours to obtain a mixed solution. Isophorone diisocyanate was then added dropwise to ensure the stoichiometric ratio of NCO and OH. The temperature was adjusted to 65°C for polymerization reaction for 7 hours. The mixture was then precipitated in excess water and washed to remove solvent A. The mixture was then dried in an oven at 70°C to obtain a polyurethane for standby use.

[0061] (4) The reinforcing filler, modified lignin and pretreated plant fiber were mixed and added to tetrachloroethane, and then castor oil was added and treated under 600W ultrasound for 10 minutes. Then the above-mentioned polyurethane was added and stirred thoroughly to obtain a mixed slurry, wherein the mass ratio of the reinforcing filler, modified lignin, pretreated plant fiber, castor oil, polyurethane, and tetrachloroethane was 0.3:0.1:1.1:0.2:7:7.

[0062] (5) Select nylon non-woven fabric with a thickness of 2.0 mm as the base material, pour the above mixed slurry into the mold box, the thickness of the mixed slurry in the mold box is 1.0 mm, then cover the slurry with non-woven fabric of the same size as the bottom of the mold, shake it slightly until the mixed slurry is fully in contact with the non-woven fabric, then heat it to 80 ° C and dry it for 18 hours, then take out the non-woven fabric, and continue to pour 1.5 mm of mixed slurry into the mold, then cover the other side of the non-woven fabric on the mixed slurry, and then place 150 g / cm 2 The plate was pressed, and then the temperature was adjusted to 80°C and dried for 24 hours to obtain a chemical mechanical polishing polyurethane material.

[0063] Detection:

[0064] The performance of the chemical mechanical polishing polyurethane materials prepared in Example 1 and Comparative Examples 1-4 was tested on a WDW-50 electronic universal testing machine:

[0065] 1. Hardness test: Shore hardness test is used according to the national standard GB / T 2411-2008. The samples are placed at 10℃, 25℃, and 50℃ for 30 minutes and then tested using a Shore hardness tester. Each sample is tested at least five points on its surface and the average value is taken. The hardness of each group of samples is shown in Table 2 below:

[0066]

[0067] As can be seen from the above table, the addition of pretreated plant fibers and modified lignin in the examples can effectively reduce the magnitude of the change in hardness of the material when heated, improve the thermal stability of the material, and ensure the polishing and grinding effect of the material under various conditions.

[0068] 2. Wear resistance test:

[0069] After each group of chemically mechanically polished polyurethane materials were fixed, the surface was polished using a grinding wheel equipped with 1,000-grit sandpaper at a speed of 3,000 rpm for 10 minutes. During the polishing process, the contact pressure was kept at 0.025 MPa, and clean water was used as the coolant. The mass loss rate of each group of materials after polishing was measured. The specific results are shown in Table 3 below:

[0070]

[0071] It can be seen from Table 3 above that the material prepared in Example 1 has good wear resistance and can effectively reduce the loss during the polishing process.

[0072] 3. Brush wire deformation resistance test:

[0073] The polyurethane materials of Example 1 and Comparative Examples 1-4 were cut and polished to form straight bristles with a diameter of 2.5±0.1 mm and a length of 5 cm. Each group of 5 bristles was set up, and each bristle was completely fixed at 90° using a mold. The bristles were then left to stand at 20°C, 30°C, and 50°C for 10 hours. The bristles were then removed and one end of the bristles was picked up. The bristles were vertically suspended at room temperature for 30 minutes, and then the deformation of the bristles was observed and the deformation rate was recorded.

[0074] The calculation formula of deformation rate is:

[0075] Deformation rate % = (a / 90) × 100%;

[0076] Where a is the angle between the straight line connecting the lower endpoint and the upper endpoint when the bristles are suspended and the vertical line segment.

[0077] The specific results are shown in Table 4 below:

[0078]

[0079] It can be seen from the above table that the bristles prepared in Example 1 have better anti-deformation effect than those prepared in Comparative Examples 1-4.

[0080] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply the existence of any such actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article, or device comprising a series of elements includes not only those elements, but also other elements not explicitly listed, or elements inherent to such process, method, article, or device. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or device comprising the element.

[0081] The above embodiments are only used to illustrate the technical solutions of the present disclosure, rather than to limit them. Although the present disclosure has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present disclosure.

Claims

1. A process for preparing a highly durable chemical mechanical polishing polyurethane material, characterized in that: The polyurethane material is obtained by setting a reinforced polyurethane material on both sides of a non-woven fabric and drying it, and the specific preparation process includes the following steps: (1) Plant fiber pretreatment: Select plant fibers and cut them into short pieces after drying, then acid-base modify them, and then dry them to obtain pretreated plant fibers for use. The acid-base modification method is to first soak them in a solution with a pH of 4.5-5.0 for 40-60 minutes, then adjust the pH to 9.0, heat them to 55-60°C and continue soaking for 20-40 minutes, then take them out, wash them to neutrality, and then dry them; (2) Lignin pretreatment: The lignin is steam-exploded and then dried to obtain modified lignin for later use, and the lignin steam explosion method is to steam-explode the lignin at a pressure of 2 MPa and a temperature of 121°C for 60-65 seconds, and then dried at a temperature of 60°C to constant weight; (3) Preparation of polyurethane: poly(1,4-butylene adipate) diol, dibutyltin dilaurate and bis(4-hydroxyphenyl) disulfide are dried and mixed, and solvent A is added and heated to dissolve to obtain a mixed solution, and isophorone diisocyanate is then added dropwise to carry out polymerization reaction, and solvent A is removed and dried to obtain polyurethane for use; (4) Mixing: The reinforcing filler, modified lignin and pretreated plant fiber are mixed and added to solvent B, castor oil is added and ultrasonically homogenized, and then the polyurethane and stannous octoate are added and stirred thoroughly to obtain a mixed slurry for use; (5) Coating: Pour the mixed slurry into the mold box and cover it with non-woven fabric. Slightly shake until the mixed slurry is fully in contact with the non-woven fabric, then heat and dry. After drying, take out the non-woven fabric and pour the mixed slurry into the mold box again. Then cover the non-woven fabric with the other side facing down on the slurry. Finally, place a non-woven fabric with a weight of 100-200g / cm 2 The board is continued to dry, then washed with water, and the surface is polished smooth after drying to obtain a highly durable chemical mechanical polishing polyurethane material.

2. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, characterized in that: The non-woven fabric has a thickness of 1.5-2.5 mm, and after the reinforced polyurethane material is arranged on both sides of the non-woven fabric, the total thickness is 3.0-3.5 mm.

3. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, characterized in that: In the step (1), the plant fiber is any one of ramie fiber and coconut fiber or a combination of two thereof, and the length of the chopped plant fiber is 1-2 cm.

4. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, wherein: In the step (3), the mass ratio of poly(1,4-butylene adipate) diol, dibutyltin dilaurate, and bis(4-hydroxyphenyl) disulfide is 20:0.36:5, and isophorone diisocyanate is added according to the stoichiometric amount of NCO and OH, etc., and the solvent A is obtained by mixing 1,4-dioxane and N,N-dimethylformamide in a mass ratio of 1:

3.

5. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, characterized in that: The temperature for heating and dissolving in step (3) is 60°C, the temperature for polymerization reaction is 65°C, and the polymerization reaction time is 6-8h.

6. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, characterized in that: In step (4), the reinforcing filler is a mixture of nano-titanium dioxide powder, nano-calcium carbonate powder, and layered graphite in a mass ratio of 1:2:1, and the solvent B is tetrachloroethane.

7. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, characterized in that: In the step (4), the mass ratio of the reinforcing filler, the modified lignin, the pretreated plant fiber, the castor oil, the polyurethane, the stannous octoate and the solvent B is 0.2-0.4: 0.1-0.2: 1-1.2: 0.1-0.2: 7: 0.05-0.08:

7.

8. The process for preparing a highly durable chemical mechanical polishing polyurethane material according to claim 1, wherein: The temperature for heating and drying in step (5) is 70-90°C.

9. A preparation process for a highly durable chemical mechanical polishing polyurethane polishing cleaning brush, characterized in that: The bristles of the cleaning brush are made of a highly durable chemical mechanical polishing polyurethane material prepared by the preparation process as claimed in claim 1, which is cut and polished to a required diameter before being installed on the brush disc.

Citation Information

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