CN116494149B - Preparation process of ceramic resin bonding agent diamond grinding wheel - Google Patents

Preparation process of ceramic resin bonding agent diamond grinding wheel Download PDF

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CN116494149B
CN116494149B CN202310609027.XA CN202310609027A CN116494149B CN 116494149 B CN116494149 B CN 116494149B CN 202310609027 A CN202310609027 A CN 202310609027A CN 116494149 B CN116494149 B CN 116494149B
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benzoxazine
polyimide
ceramic resin
grinding wheel
benzoxazinyl
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CN116494149A (en
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彭化蒙
张侠来
王相标
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Haian Boke Superhard Material Co ltd
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Haian Boke Superhard Material Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D18/00Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
    • B24D18/0009Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/28Resins or natural or synthetic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/28Resins or natural or synthetic macromolecular compounds
    • B24D3/32Resins or natural or synthetic macromolecular compounds for porous or cellular structure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/34Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
    • B24D3/342Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties incorporated in the bonding agent
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention relates to the technical field of grinding wheels, and discloses a preparation process of a ceramic resin bond diamond grinding wheel, which is characterized in that the usage ratio of pyromellitic anhydride to 4, 4-diaminodiphenyl methane is controlled, a polyamide acid intermediate with an anhydride group is synthesized, and then the polyamide acid intermediate reacts with hydroxyl groups of phenolic hydroxyl benzoxazine to obtain benzoxazine polyimide resin, so that a benzoxazine structure is introduced into a molecular chain of polyimide, the benzoxazine structure is used as a main body of a resin bond, and is compounded with molybdenum disulfide, carbon fiber, silicon carbide and copper powder to obtain the benzoxazine polyimide ceramic resin bond, the benzoxazine group can form a phenolic resin structure in a heat curing process, the rigidity is high, the thermosetting property is good, and the obtained ceramic resin bond diamond grinding wheel has higher abrasion ratio and grinding efficiency.

Description

Preparation process of ceramic resin bonding agent diamond grinding wheel
Technical Field
The invention relates to the technical field of grinding wheels, in particular to a preparation process of a ceramic resin bond diamond grinding wheel.
Background
The resin-based diamond grinding wheel has the advantages of high grinding efficiency, excellent self-sharpening property and the like, and is widely applied to grinding processing of materials such as glass, ceramics, alloys and the like, and the resin bonding agent mainly comprises phenolic resin, polyimide resin and the like.
The polyimide resin has good heat resistance, high strength and strong chemical stability, has wide application prospect in the grinding wheel resin bonding agent, and reports that the diamond resin grinding wheel obtained by adopting sodium hydroxide and silane coupling agent to carry out surface modification on the structural formula and compounding the structural formula with polyimide resin has excellent grinding ratio, sharpness and self-sharpening property, as in the literature 'influence of coupling agent treatment on the grinding performance of diamond resin grinding wheel'.
Patent CN115366013a, "bismaleimide resin grinding wheel for dry grinding", discloses a bismaleimide resin grinding wheel obtained by compounding modified bismaleimide resin, toughening agent polymethyl methacrylate and the like serving as raw materials with abrasive materials such as diamond and the like, silicon carbide, corundum, graphite, molybdenum disulfide, copper powder and the like, wherein toughness is improved, more uniform dispersion is achieved in the processing process, and compactness is improved.
Disclosure of Invention
(one) solving the technical problems
The invention provides a preparation process of a ceramic resin bond diamond grinding wheel with high abrasion ratio and high grinding efficiency.
(II) technical scheme
The preparation process of the ceramic resin bond diamond grinding wheel comprises the following steps: and uniformly mixing the diamond and the benzoxazine polyimide ceramic resin binder, performing heat preservation and pressure maintaining treatment in a hot press at 240-270 ℃ and at 100-130MPa, and then performing cold pressing in a cold press at 100-150MPa to obtain the ceramic resin binder diamond grinding wheel.
Preferably, the benzoxazine-based polyimide ceramic resin bonding agent comprises the following components in parts by weight: 25-35% of benzoxazinyl polyimide resin, 1-2% of molybdenum disulfide, 1-3% of carbon fiber, 3-8% of silicon carbide and the balance of copper powder.
Preferably, the preparation process of the benzoxazine-based polyimide ceramic resin bonding agent comprises the following steps:
(1) Adding pyromellitic anhydride and 4, 4-diaminodiphenyl methane into N, N-dimethylacetamide, reacting for 2-4 hours in nitrogen atmosphere to obtain a polyamic acid intermediate with an anhydride group, adding phenolic hydroxyl benzoxazine, reacting for 3-6 hours, heating and thermally curing the solution in an oven after the reaction, and grinding the thermally cured material into powder to obtain the benzoxazinyl polyimide resin.
(2) Adding benzoxazinyl polyimide resin, molybdenum disulfide, carbon fiber, silicon carbide and copper powder into liquid paraffin, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
Preferably, the molar ratio of the pyromellitic anhydride, the 4, 4-diaminodiphenylmethane and the phenolic hydroxy benzoxazine is 1.1-1.3:1:0.03-0.08.
Preferably, the heating program of the heating and heat curing is 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h in sequence.
Preferably, the preparation process of the phenolic hydroxyl benzoxazine comprises the following steps: adding triethylamine, formaldehyde solution, 4-diaminodiphenylmethane and bisphenol A into 1, 4-dioxane, controlling the molar ratio of formaldehyde to 4, 4-diaminodiphenylmethane to bisphenol A to be 4:1:2, heating and refluxing for 2-5 hours, concentrating under reduced pressure after the reaction, washing with deionized water and ethanol to obtain the phenolic hydroxy benzoxazine, wherein the structural formula is
(III) beneficial technical effects
According to the invention, the usage ratio of pyromellitic anhydride to 4, 4-diaminodiphenyl methane is controlled, a polyamide acid intermediate with an anhydride group is synthesized, and then the polyamide acid intermediate reacts with the hydroxyl of phenolic hydroxyl benzoxazine to obtain benzoxazinyl polyimide resin, so that a benzoxazinyl polyimide resin is introduced into a molecular chain of polyimide, and the benzoxazinyl polyimide resin is compounded with molybdenum disulfide, carbon fiber, silicon carbide and copper powder to obtain a benzoxazinyl polyimide ceramic resin bonding agent, wherein the benzoxazinyl polyimide resin bonding agent is compounded with molybdenum disulfide, carbon fiber, silicon carbide and copper powder, and the benzoxazinyl group can form a phenolic resin structure in the heat curing process.
Detailed Description
Example 1
(1) 7mmol of triethylamine, a solution containing 300mmol of formaldehyde, 75mmol of 4, 4-diaminodiphenyl methane and 150mmol of bisphenol A are added into 1, 4-dioxane, the mixture is heated and refluxed for 5 hours, and after the reaction, the mixture is concentrated under reduced pressure, and then washed by deionized water and ethanol to obtain the phenolic hydroxyl benzoxazine.
(2) Adding 33mmol of pyromellitic anhydride and 30mmol of 4, 4-diaminodiphenylmethane into N, N-dimethylacetamide, reacting for 4 hours in a nitrogen atmosphere to obtain a polyamide acid intermediate with an anhydride group, then adding 0.9mmol of phenolic hydroxy benzoxazine, reacting for 3 hours, heating and thermally curing the solution in an oven after the reaction, and grinding the thermally cured materials into powder at the temperature of 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h in sequence to obtain the benzoxazinyl polyimide resin.
(3) Adding 25% of benzoxazinyl polyimide resin, 2% of molybdenum disulfide, 2% of carbon fiber, 3% of silicon carbide and the balance of copper powder into liquid paraffin in weight ratio, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
(4) And uniformly mixing the diamond and the benzoxazine polyimide ceramic resin bond, performing heat preservation and pressure maintaining treatment in a hot press at 270 ℃ and 120MPa, and then performing cold pressing in a cold press at 100MPa to obtain the ceramic resin bond diamond grinding wheel.
Example 2
(1) 7mmol of triethylamine, a solution containing 300mmol of formaldehyde, 75mmol of 4, 4-diaminodiphenyl methane and 150mmol of bisphenol A are added into 1, 4-dioxane, the mixture is heated and refluxed for 2 hours, and after the reaction, the mixture is concentrated under reduced pressure, and then washed by deionized water and ethanol to obtain the phenolic hydroxyl benzoxazine.
(2) Adding 33mmol of pyromellitic anhydride and 30mmol of 4, 4-diaminodiphenylmethane into N, N-dimethylacetamide, reacting for 3 hours in a nitrogen atmosphere to obtain a polyamide acid intermediate with an anhydride group, then adding 2.4mmol of phenolic hydroxybenzooxazine, reacting for 6 hours, heating and thermally curing the solution in an oven after the reaction, and grinding the thermally cured materials into powder at the temperature of 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h in sequence to obtain the benzoxazinyl polyimide resin.
(3) Adding 30% of benzoxazinyl polyimide resin, 1% of molybdenum disulfide, 1% of carbon fiber, 8% of silicon carbide and the balance of copper powder into liquid paraffin in weight ratio, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
(4) And uniformly mixing the diamond and the benzoxazine polyimide ceramic resin bond, performing heat preservation and pressure maintaining treatment in a hot press at 270 ℃ and 120MPa, and then performing cold pressing in a cold press at 100MPa to obtain the ceramic resin bond diamond grinding wheel.
Example 3
(1) 7mmol of triethylamine, a solution containing 300mmol of formaldehyde, 75mmol of 4, 4-diaminodiphenyl methane and 150mmol of bisphenol A are added into 1, 4-dioxane, the mixture is heated and refluxed for 3 hours, and after the reaction, the mixture is concentrated under reduced pressure, and then washed by deionized water and ethanol to obtain the phenolic hydroxyl benzoxazine.
(2) 39mmol of pyromellitic anhydride and 30mmol of 4, 4-diaminodiphenylmethane are added into N, N-dimethylacetamide to react for 3 hours in a nitrogen atmosphere to obtain a polyamide acid intermediate with an anhydride group, then 2mmol of phenolic hydroxyl benzoxazine is added to react for 6 hours, the solution is heated and thermally cured in an oven after the reaction, the heating procedures are sequentially 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h, and the thermally cured material is ground into powder to obtain the benzoxazinyl polyimide resin.
(3) Adding 30% of benzoxazinyl polyimide resin, 2% of molybdenum disulfide, 2% of carbon fiber, 5% of silicon carbide and the balance of copper powder into liquid paraffin in weight ratio, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
(4) And uniformly mixing the diamond and the benzoxazine polyimide ceramic resin bond, performing heat preservation and pressure maintaining treatment in a hot press at 240 ℃ and 100MPa, and then performing cold pressing in a cold press at 150MPa to obtain the ceramic resin bond diamond grinding wheel.
Example 4
(1) 7mmol of triethylamine, a solution containing 300mmol of formaldehyde, 75mmol of 4, 4-diaminodiphenyl methane and 150mmol of bisphenol A are added into 1, 4-dioxane, the mixture is heated and refluxed for 5 hours, and after the reaction, the mixture is concentrated under reduced pressure, and then washed by deionized water and ethanol to obtain the phenolic hydroxyl benzoxazine.
(2) Adding 35mmol of pyromellitic anhydride and 30mmol of 4, 4-diaminodiphenylmethane into N, N-dimethylacetamide, reacting for 4 hours in a nitrogen atmosphere to obtain a polyamide acid intermediate with an anhydride group, then adding 1.5mmol of phenolic hydroxy benzoxazine, reacting for 4 hours, heating and thermally curing the solution in an oven after the reaction, and grinding the thermally cured materials into powder at the temperature of 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h in sequence to obtain the benzoxazinyl polyimide resin.
(3) Adding 35% of benzoxazinyl polyimide resin, 2% of molybdenum disulfide, 2% of carbon fiber, 3% of silicon carbide and the balance of copper powder into liquid paraffin in weight ratio, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
(4) And uniformly mixing the diamond and the benzoxazine polyimide ceramic resin bond, performing heat preservation and pressure maintaining treatment in a hot press at the temperature of 250 ℃ and the pressure of 120MPa, and then performing cold pressing in a cold press at the pressure of 140MPa to obtain the ceramic resin bond diamond grinding wheel.
Example 5
(1) 7mmol of triethylamine, a solution containing 300mmol of formaldehyde, 75mmol of 4, 4-diaminodiphenyl methane and 150mmol of bisphenol A are added into 1, 4-dioxane, the mixture is heated and refluxed for 5 hours, and after the reaction, the mixture is concentrated under reduced pressure, and then washed by deionized water and ethanol to obtain the phenolic hydroxyl benzoxazine.
(2) 39mmol of pyromellitic anhydride and 30mmol of 4, 4-diaminodiphenylmethane are added into N, N-dimethylacetamide to react for 3 hours in a nitrogen atmosphere to obtain a polyamide acid intermediate with an anhydride group, then 1.5mmol of phenolic hydroxy benzoxazine is added to react for 4 hours, the solution is heated and thermally cured in an oven after the reaction, the heating program is sequentially 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h, and the thermally cured material is ground into powder to obtain the benzoxazinyl polyimide resin.
(3) Adding 25% of benzoxazinyl polyimide resin, 1% of molybdenum disulfide, 2% of carbon fiber, 8% of silicon carbide and the balance of copper powder into liquid paraffin in weight ratio, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
(4) And uniformly mixing the diamond and the benzoxazine polyimide ceramic resin bond, performing heat preservation and pressure maintaining treatment in a hot press at 240 ℃ and 130MPa, and then performing cold pressing in a cold press at 100MPa to obtain the ceramic resin bond diamond grinding wheel.
Example 6
(1) 7mmol of triethylamine, a solution containing 300mmol of formaldehyde, 75mmol of 4, 4-diaminodiphenyl methane and 150mmol of bisphenol A are added into 1, 4-dioxane, the mixture is heated and refluxed for 2 hours, and after the reaction, the mixture is concentrated under reduced pressure, and then washed by deionized water and ethanol to obtain the phenolic hydroxyl benzoxazine.
(2) 39mmol of pyromellitic anhydride and 30mmol of 4, 4-diaminodiphenylmethane are added into N, N-dimethylacetamide to react for 4 hours in a nitrogen atmosphere to obtain a polyamide acid intermediate with an anhydride group, then 2.4mmol of phenolic hydroxy benzoxazine is added to react for 5 hours, the solution is heated and thermally cured in an oven after the reaction, the heating program is sequentially 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h, and the thermally cured material is ground into powder to obtain the benzoxazinyl polyimide resin.
(3) Adding 35% of benzoxazinyl polyimide resin, 1.5% of molybdenum disulfide, 1% of carbon fiber, 5% of silicon carbide and the balance of copper powder into liquid paraffin in weight ratio, and uniformly dispersing to obtain the benzoxazinyl polyimide ceramic resin binder.
(4) And uniformly mixing the diamond and the benzoxazine polyimide ceramic resin bond, performing heat preservation and pressure maintaining treatment in a hot press at 270 ℃ and under 100MPa, and then performing cold pressing in a cold press at 120MPa to obtain the ceramic resin bond diamond grinding wheel.
The grinding ratio of the ceramic resin bond diamond grinding wheel prepared in each example is maximum to obtain 348.6. The abrasion ratio is large, and the grinding efficiency is high.

Claims (3)

1. The preparation process of the ceramic resin bond diamond grinding wheel is characterized by comprising the following steps of: the preparation process comprises the following steps: uniformly mixing diamond and benzoxazine polyimide ceramic resin binder, carrying out heat preservation and pressure maintaining treatment in a hot press at 240-270 ℃ and 100-130MPa, and then carrying out cold pressing in a cold press at 100-150MPa to obtain a ceramic resin binder diamond grinding wheel;
the preparation process of the benzoxazine-based polyimide ceramic resin bonding agent comprises the following steps:
(1) Adding pyromellitic anhydride and 4, 4-diaminodiphenyl methane into N, N-dimethylacetamide, reacting for 2-4 hours in nitrogen atmosphere to obtain a polyamic acid intermediate with an anhydride group, and then adding phenolic hydroxy benzoxazine, wherein the molar ratio of the pyromellitic anhydride to the 4, 4-diaminodiphenyl methane to the phenolic hydroxy benzoxazine is 1.1-1.3:1:0.03-0.08; reacting for 3-6h, heating and thermally curing the solution in an oven after the reaction, and grinding the thermally cured material into powder to obtain the benzoxazinyl polyimide resin;
(2) Adding benzoxazinyl polyimide resin, molybdenum disulfide, carbon fiber, silicon carbide and copper powder into liquid paraffin, and uniformly dispersing to obtain a benzoxazinyl polyimide ceramic resin binder;
the preparation process of the phenolic hydroxyl benzoxazine comprises the following steps: adding triethylamine, formaldehyde solution, 4-diaminodiphenyl methane and bisphenol A into 1, 4-dioxane, controlling the molar ratio of formaldehyde to 4, 4-diaminodiphenyl methane to bisphenol A to be 4:1:2, heating and refluxing for 2-5 hours, concentrating under reduced pressure after the reaction, washing with deionized water and ethanol, and obtaining the phenolic hydroxy benzoxazine.
2. The process for preparing the ceramic resin bond diamond grinding wheel according to claim 1, which is characterized in that: the benzoxazine-based polyimide ceramic resin bonding agent comprises the following components in parts by weight: 25-35% of benzoxazinyl polyimide resin, 1-2% of molybdenum disulfide, 1-3% of carbon fiber, 3-8% of silicon carbide and the balance of copper powder.
3. The process for preparing the ceramic resin bond diamond grinding wheel according to claim 1, which is characterized in that: the heating program of the heating and heat curing is 100 ℃/1h, 180 ℃/3h, 240 ℃/3h and 280 ℃/2h in sequence.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103755987A (en) * 2014-01-20 2014-04-30 江苏冰城电材股份有限公司 Preparation method for heat-resisting and high-transparence polyimide thin film
CN104149037A (en) * 2014-07-31 2014-11-19 桂林创源金刚石有限公司 Resinoid- and ceramic-binder diamond grinding wheel
CN104861650A (en) * 2015-06-10 2015-08-26 花秀兵 Heat-resistant benzoxazine resin and preparation method thereof
KR20160095959A (en) * 2015-02-04 2016-08-12 주식회사 엘지화학 Adhesive resin composition, adhesive film, and flexible metal laminate
CN109863215A (en) * 2016-10-26 2019-06-07 科思创德国股份有限公司 The low viscosity polyisocyanates based on TDI with isocyanurate group

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103755987A (en) * 2014-01-20 2014-04-30 江苏冰城电材股份有限公司 Preparation method for heat-resisting and high-transparence polyimide thin film
CN104149037A (en) * 2014-07-31 2014-11-19 桂林创源金刚石有限公司 Resinoid- and ceramic-binder diamond grinding wheel
KR20160095959A (en) * 2015-02-04 2016-08-12 주식회사 엘지화학 Adhesive resin composition, adhesive film, and flexible metal laminate
CN104861650A (en) * 2015-06-10 2015-08-26 花秀兵 Heat-resistant benzoxazine resin and preparation method thereof
CN109863215A (en) * 2016-10-26 2019-06-07 科思创德国股份有限公司 The low viscosity polyisocyanates based on TDI with isocyanurate group

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含硅、氮、硼元素耐高温芳基乙炔树脂 及其复合材料的研究;宋宁;《华东理工大学》;第5页 *

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