CN112625218B - Epoxy resin for cutting water-resistant silicon rod and preparation method thereof - Google Patents
Epoxy resin for cutting water-resistant silicon rod and preparation method thereof Download PDFInfo
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- CN112625218B CN112625218B CN202011501984.3A CN202011501984A CN112625218B CN 112625218 B CN112625218 B CN 112625218B CN 202011501984 A CN202011501984 A CN 202011501984A CN 112625218 B CN112625218 B CN 112625218B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/66—Mercaptans
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The application discloses an epoxy resin for cutting a water-resistant silicon rod in the technical field of epoxy adhesives, and relates to a water-resistant epoxy resin which can be widely applied to temporary bonding for cutting a silicon rod, and the epoxy resin comprises a component A and a component B, wherein the component A comprises a high-functionality epoxy resin, the component B comprises a modified polymercaptan and a long-carbon-chain silane coupling agent, and the average functionality of the high-functionality epoxy resin is more than or equal to 3; the modified polymercaptan is obtained by modifying a polythiol curing agent by using isocyanatopropyl triethoxysilane or isocyanatopropyl trimethoxysilane as a modifying agent. According to the method, the isocyanate silane coupling agent is adopted to modify the commercial polymeric thiol curing agent, the modified curing agent system is added with the long-carbon-chain silane coupling agent, and meanwhile, the high-functionality epoxy resin is introduced into the colloid system, so that the water-resistant bonding performance of the colloid system in the washing process is improved while the rapid degumming of water is ensured, and unnecessary losses such as degumming, sheet falling and the like in the cleaning process are prevented.
Description
Technical Field
The invention belongs to the technical field of epoxy resin adhesives, and particularly relates to epoxy resin for cutting a water-resistant silicon rod and a preparation method thereof.
Background
In recent years, the photovoltaic industry has been rapidly developed and gradually becomes the main body of world energy supply, and due to environmental protection and replaceability, solar photovoltaic power generation is expected to account for more than 60% of the total world power supply in 2050. Therefore, the photovoltaic industry plays an important role in the field of new energy, and the market prospect is very considerable.
The monocrystalline silicon wafer is a key technology at the upstream of photovoltaic power generation, is also a key material of a semiconductor device, and accounts for more than 90% of the semiconductor industry of integrated circuits, so the monocrystalline silicon rod cutting glue plays an important role in the monocrystalline silicon wafer industry. The existing silicon rod cutting technology is only limited to degumming performance after cutting, namely, smooth degumming can be realized under the condition of water boiling or acid boiling; for example, patent CN109880567A is disclosed, including: the component A comprises: glycidyl ester type epoxy resin, general bisphenol A epoxy resin, glycidyl ether, a filler, a defoaming agent, an anti-settling agent and a coupling agent; and the component B comprises: modified polythiol, self-made m-xylylenediamine prepolymer, accelerant, filler, defoaming agent and anti-settling agent, although can accomplish the problem of not adding sour poaching and come unstuck, and the temperature of coming unstuck is also lower, can guarantee certain silicon chip cutting requirement, spray to cutting fluid in cutting process also has certain water resistance, but this cutting glue is washing, the bonding force decline range is too big in cleaning process such as ultrasonic wave washing, and the colloid proportion of coming unstuck is obviously too much after wasing, on this basis, prior art needs provide a colloid with certain water resistance, satisfy the demand of washing cleaning process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a product which has better adhesive property and longer water-resistant time and can be quickly boiled and degummed in the water washing process after cutting.
One of the purposes of the invention is to provide a water-resistant epoxy resin for cutting a silicon rod, which comprises a component A and a component B, wherein the component A comprises a high-functionality epoxy resin, the component B comprises a modified polymeric mercaptan and a long-carbon-chain silane coupling agent, and the average functionality of the high-functionality epoxy resin is more than or equal to 3; the modified polymeric mercaptan is obtained by modifying a polythiol curing agent by using isocyanatopropyl triethoxysilane or isocyanatopropyl trimethoxysilane as a modifying agent.
Preferably, the polythiol curing agent has an active hydrogen equivalent of 150 to 240, and the modification method of the modified polymercaptan comprises the following steps: modifying agent and polythiol curing agent according to the weight ratio of 0.1-5: 100, and fully reacting under the conditions of vacuum or nitrogen atmosphere and the temperature of 25-35 ℃, wherein the reaction formula is shown as follows:
preferably, the long carbon chain silane coupling agent satisfies at least one of the following structures;
wherein n is more than or equal to 7; r 1 ,R 2 ,R 3 Is methyl or ethyl.
More specifically, the component A and the component B comprise the following substances in parts by weight:
and (2) component A:
and the component B comprises:
preferably, the bisphenol A type epoxy resin is at least one of easy-mixing, namely, good-compatibility resin such as E-20, E-44, E-51, E-54 and E-56; the high-functionality epoxy resin is at least one of F-51, F-44, F-50 and F-48.
Preferably, the toughening agent is a reactive diluent containing a monofunctional group or a difunctional group, and specifically is a reactive diluent capable of adjusting the viscosity and toughness of a system, such as at least one of 1, 4-butanediol diglycidyl ether, 1, 6-hexanediol diglycidyl ether or dodecaglycidyl ether.
Preferably, the accelerator is a curing accelerator capable of adjusting the operation time of the system, such as at least one of triethylamine, 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), pyridine, resorcinol, m-cresol or phenol; the amine value of the fatty amine is more than or equal to 500mgKOH/g.
Preferably, the filler is at least one of calcium carbonate, silica micropowder, talcum powder, alumina, aluminum hydroxide or common silica.
Preferably, the anti-settling agent is at least one of fumed silica, organic bentonite or hydrogenated castor oil.
The invention also aims to provide a preparation method of the epoxy resin for cutting the water-resistant silicon rod, which comprises the following steps:
(1) Preparation of a component A: according to the material composition of the component A, according to the weight ratio, adding bisphenol A type epoxy resin, high functionality epoxy resin, a toughening agent, a filler, an anti-settling agent and a defoaming agent into a planetary stirrer, and dispersing and uniformly mixing under a vacuum condition and then discharging to obtain the component A;
(2) B, preparation of a component: according to the weight ratio of the material composition of the component B, stirring and dispersing the modified polymeric mercaptan and the long carbon chain coupling agent for 30 minutes at normal temperature under the closed condition of 55 percent RH, sequentially adding fatty amine, an accelerator, a filler, a defoaming agent and an anti-settling agent into dispersing equipment, and dispersing and mixing uniformly under the vacuum condition to obtain the component B;
(3) Mixing: the component A and the component B are mixed according to the weight ratio of A: b =1: 0.8-2, and obtaining the epoxy resin for cutting the water-resistant silicon rod.
The epoxy resin provided by the invention is not only suitable for cutting silicon wafers and jewels, but also suitable for temporarily fixing and bonding workpieces.
The invention has the beneficial effects that: 1. according to the invention, the commercially available polythiol is modified by adopting the isocyanate silane coupling agent, the modified polythiol retains the main performance of mercaptan, and meanwhile, the silane coupling agent structure is introduced into the molecular structure, so that siloxane can generate hydrolysis reaction with hydroxyl in the system, thus the adhesion to the surface of the base material is increased, and the water resistance of the system is improved; and because the isocyanate coupling agent only reacts a small part of active hydrogen groups in the polythiol system, the system has the performance of boiling degumming, namely the balance between water resistance and degumming performance is controlled. 2. In the production process, firstly, the modified polymeric mercaptan reacts with the long-carbon-chain silane coupling agent under the condition of containing a trace amount of moisture, so that the long-carbon-chain silane coupling agent and siloxane in the structure of the modified polymeric mercaptan are subjected to partial hydrolytic polycondensation, and the long-carbon-chain structure is introduced into the molecules of the modified polymeric mercaptan, namely, the long-carbon-chain hydrophobic structure is fused, so that the water resistance is further improved, and the water-resistant bonding performance in the cleaning process after slicing is improved. 3. By using the general bisphenol A epoxy resin and the high-functionality epoxy resin in a matching way, the crosslinking density of the system is improved by increasing the crosslinking points of the system, the colloid is endowed with higher hardness and better adhesive property, and the cutting quality is favorably improved.
Detailed Description
The following is further detailed by way of specific embodiments:
example 1
The water-resistant adhesive stick epoxy resin comprises the following raw materials in parts by weight:
and (2) component A: 40 parts of bisphenol A type epoxy resin, 1 part of high-functionality epoxy resin, 0.1 part of toughening agent, 30 parts of filler, 0.01 part of anti-settling agent and 0.01 part of defoaming agent;
and the component B comprises: 30 parts of modified polymer mercaptan, 0.05 part of long carbon chain silane coupling agent, 0.05 part of fatty amine, 1 part of accelerator, 20 parts of filler, 0.01 part of defoaming agent and 0.01 part of anti-settling agent;
wherein the bisphenol A epoxy resin is E-51, the high-functionality epoxy resin is F-51, the toughening agent is 1, 4-butanediol diglycidyl ether, and the modified polymeric mercaptan is IPTS and the commercial polymeric mercaptan in a weight ratio of 0.1:100, mixing and fully reacting;
the long carbon chain silane coupling agent is n-octyl trimethoxy silane and n-dodecyl trimethoxy silane in a weight ratio of 1:1, mixing;
the filler is calcium carbonate, the accelerator is DMP-30, the defoaming agent is an organic silicon defoaming agent, and the anti-settling agent is fumed silica.
The mixing method comprises the following steps: respectively uniformly mixing the component A and the component B in a dispersion machine, filtering and subpackaging; when in use, the components A and B are mixed according to the ratio of 1:1 proportion, and bonding between the adhesive and the adhesive plate.
Example 2
The component A comprises: 65 parts of bisphenol A epoxy resin, 5 parts of high-functionality epoxy resin, 0.5 part of toughening agent, 45 parts of filler, 2 parts of anti-settling agent and 1 part of defoaming agent;
and the component B comprises: 60 parts of modified polymeric mercaptan, 2 parts of long-carbon-chain silane coupling agent, 1 part of fatty amine, 5 parts of accelerator, 35 parts of filler, 2 parts of defoaming agent and 1 part of anti-settling agent;
wherein the bisphenol A epoxy resin is prepared by mixing E-51 and E-44 in a weight ratio of 2:1, mixing, wherein the high-functionality epoxy resin is F-44, the toughening agent is 1, 4-butanediol diglycidyl ether, and the modified polymeric mercaptan is IPTS and commercial polymeric mercaptan in a weight ratio of 2:100, mixing and fully reacting;
the long carbon chain silane coupling agent is n-hexadecyl trimethoxy silane and n-dodecyl trimethoxy silane in the weight ratio of 1:1, mixing;
the filler is calcium carbonate and silicon micropowder according to the weight ratio of 1:0.5, and the promoter is DMP-30 and triethylamine according to the weight ratio of 1:0.1, the defoaming agent is an organic silicon defoaming agent, and the anti-settling agent is fumed silica.
The mixing method comprises the following steps: respectively and uniformly mixing the component A and the component B in a dispersion machine, filtering and subpackaging; when in use, the components A and B are mixed according to the ratio of 1:1.1, and bonding between the adhesive and the adhesive plate.
Example 3
The component A comprises: 50 parts of bisphenol A type epoxy resin, 3 parts of high-functionality epoxy resin, 0.3 part of toughening agent, 35 parts of filler, 0.12 part of anti-settling agent and 0.5 part of defoaming agent;
and B component: 48 parts of modified polymeric mercaptan, 1 part of long carbon chain silane coupling agent, 0.14 part of fatty amine, 4 parts of accelerator, 24 parts of filler, 0.08 part of defoaming agent and 0.6 part of anti-settling agent;
wherein, the bisphenol A type epoxy resin is prepared by mixing E-56 and E-44 in a weight ratio of 5:1, mixing, wherein the high-functionality epoxy resin is F-50, the toughening agent is 1, 6-hexanediol diglycidyl ether, and the modified polymeric mercaptan is IPTS and commercial polymeric mercaptan in a weight ratio of 2.5:100, mixing and fully reacting;
the long carbon chain silane coupling agent is n-octyl trimethoxy silane and n-dodecyl trimethoxy silane in a weight ratio of 1:2, mixing;
the filler is calcium carbonate and silicon micropowder according to the weight ratio of 1:1, mixing an accelerant triethylamine and pyridine according to a weight ratio of 1:0.8, the defoaming agent is an organic silicon defoaming agent, and the anti-settling agent is hydrogenated castor oil.
The mixing method comprises the following steps: respectively uniformly mixing the component A and the component B in a dispersion machine, filtering and subpackaging; when in use, the components A and B are mixed according to the ratio of 1: mixing at a ratio of 0.8, and bonding between the adhesive and the bonding plate.
Example 4
The component A comprises: 54 parts of bisphenol A epoxy resin, 4 parts of high-functionality epoxy resin, 0.4 part of toughening agent, 40 parts of filler, 1 part of anti-settling agent and 0.08 part of defoaming agent;
and B component: 35 parts of modified polymeric mercaptan, 1.5 parts of long carbon chain silane coupling agent, 0.6 part of fatty amine, 3 parts of accelerator, 30 parts of filler, 0.9 part of defoaming agent and 0.18 part of anti-settling agent;
wherein the bisphenol A type epoxy resin is prepared by mixing E-54 and E-51 according to the weight ratio of 1:0.5, and mixing, wherein the high-functionality epoxy resin is F-51 and F-44 according to the weight ratio of 1:0.8, and the toughening agent is dodecyl glycidyl ether; the modified polymeric mercaptan is IPTS and commercial polymeric mercaptan in a weight ratio of 0.5:100, mixing and fully reacting;
the long-carbon-chain silane coupling agent is n-dodecyl triethoxysilane and n-hexadecyl triethoxysilane with the weight ratio of 1:0.6 mixing;
the filler is calcium carbonate and talcum powder according to the weight ratio of 1:0.2, mixing the accelerator DMP-30 and resorcinol according to the weight ratio of 1:0.5, the defoaming agent is organic silicon defoaming agent, and the anti-settling agent is organic bentonite.
The mixing method comprises the following steps: respectively and uniformly mixing the component A and the component B in a dispersion machine, filtering and subpackaging; when in use, the components A and B are mixed according to the proportion of 1:1.5, and bonding the mixture between the adhesive and the adhesive plate.
Example 5
And (2) component A: 46 parts of bisphenol A epoxy resin, 2 parts of high-functionality epoxy resin, 0.2 part of toughening agent, 40 parts of filler, 1.4 parts of anti-settling agent and 0.8 part of defoaming agent;
and B component: 52 parts of modified polymeric mercaptan, 1.5 parts of long carbon chain silane coupling agent, 0.8 part of fatty amine, 3 parts of accelerator, 32 parts of filler, 1.5 parts of defoaming agent and 0.7 part of anti-settling agent;
wherein the bisphenol A type epoxy resin is E-56 and E-44 according to the weight ratio of 1:0.5, and F-50 and F-48 are mixed, wherein the weight ratio of the high-functionality epoxy resin to the high-functionality epoxy resin is 1:0.2, and the toughening agent is 1, 4-butanediol diglycidyl ether and 1, 6-hexanediol diglycidyl ether in a weight ratio of 1:0.7, wherein the weight ratio of the modified polymer mercaptan to the commercial polymer mercaptan Is (IPTS) 3.5:100, mixing and fully reacting;
the long carbon chain silane coupling agent is n-octyl triethoxysilane and n-dodecyl triethoxysilane according to the weight ratio of 1:0.7 mixing;
the filler is calcium carbonate and alumina according to the weight ratio of 1:0.6, mixing the accelerant DMP-30 and m-cresol according to the weight ratio of 1:0.4, the defoaming agent is a silicone defoaming agent, and the anti-settling agent is hydrogenated castor oil.
The mixing method comprises the following steps: respectively uniformly mixing the component A and the component B in a dispersion machine, filtering and subpackaging; when in use, the components A and B are mixed according to the ratio of 1: mixing at a ratio of 0.8, and bonding between the adhesive and the bonding plate.
Example 6
And (2) component A: 45 parts of bisphenol A epoxy resin, 6 parts of high-functionality epoxy resin, 0.5 part of toughening agent, 60 parts of filler, 1.5 parts of anti-settling agent and 0.75 part of defoaming agent;
and B component: 58 parts of modified polymeric mercaptan, 1.8 parts of long carbon chain silane coupling agent, 0.5 part of fatty amine, 4 parts of accelerator, 45 parts of filler, 1.7 parts of defoaming agent and 0.9 part of anti-settling agent;
wherein the bisphenol A type epoxy resin is E-51, E-54 and E-44 according to the weight ratio of 1:0.5:0.1, and the high functionality epoxy resin is F-51, F-48 and F-44 in a weight ratio of 1:0.2:0.1, and the toughening agent is 1, 6-hexanediol diglycidyl ether and dodecaglycidyl ether in a weight ratio of 1:0.8, mixing the modified polymer thiol with IPTS and commercial polymer thiol according to the weight ratio of 5:100, mixing and fully reacting;
the long carbon chain silane coupling agent is n-dodecyl trimethoxy silane and n-hexadecyl triethoxy silane in a weight ratio of 1:0.5 mixing;
the filler is calcium carbonate, aluminum hydroxide and common silicon dioxide according to the weight ratio of 1:0.4:0.2, mixing the promoter DMP-30 and the phenol according to the weight ratio of 1:0.5, the defoamer is organic silicon defoamer, and the anti-settling agent is organic bentonite.
The mixing method comprises the following steps: respectively and uniformly mixing the component A and the component B in a dispersion machine, filtering and subpackaging; when in use, the components A and B are mixed according to the ratio of 1:2, and bonding the mixture between the adhesive and the adhesive plate.
Comparative example 1
The preparation was carried out in accordance with the composition and method of example 3, except that the high-functional epoxy resin and the long-carbon-chain silane coupling agent were not added.
Comparative example 2
Except no high-functionality epoxy resin and long carbon chain silane coupling agent, the adhesive is prepared by adopting the conventional commercial polymeric mercaptan according to the published Chinese patent CN109880567A diamond wire silicon slice adhesive rod and the preparation method:
the paint specifically comprises the following raw materials in parts by weight:
the component A comprises: 75 parts of bisphenol A epoxy resin, 10 parts of glycidyl ester epoxy resin, 5 parts of glycidyl ether, 60 parts of filler, 3 parts of coupling agent, 5 parts of anti-settling agent and 3 parts of defoaming agent;
and B component: 50 parts of modified polymeric mercaptan, 5 parts of self-made m-xylylenediamine, 10 parts of an accelerator, 40 parts of a filler, 3 parts of a defoaming agent and 5 parts of an anti-settling agent;
wherein the self-made m-xylylenediamine prepolymer is a product disclosed in the patent No. CN 103665327B; the bisphenol A type epoxy resin is E-51, the glycidyl ester type epoxy resin is glycidyl methacrylate, the glycidyl ether is 1, 4-butanediol diglycidyl ether, and the modified polymeric mercaptan is polythiol 3800 according to a weight ratio of 1:1, mixing to obtain; the coupling agent is KH-550;
the filler is calcium carbonate, the accelerator is DMP-30, the defoamer is BKY-072, and the anti-settling agent is fumed silica.
The preparation method comprises the following steps:
preparation of a component A: adding 75 parts of bisphenol A type epoxy resin, 10 parts of glycidyl ester type epoxy resin, 5 parts of glycidyl ether, 60 parts of filler, 3 parts of coupling agent, 5 parts of anti-settling agent and 3 parts of defoaming agent into a planetary stirrer according to the mass ratio, controlling the temperature to be about 45 ℃ under the vacuum condition, stirring for 1-1.5, discharging and sealing to obtain a component A;
b, preparation of a component: 50 parts of modified polymer mercaptan, 5 parts of self-made m-xylylenediamine, 10 parts of an accelerator, 40 parts of a filler, 3 parts of a defoaming agent and 5 parts of an anti-settling agent are mixed according to the mass ratio; adding into a planetary stirrer, stirring at about 45 deg.C under vacuum for 1-1.5 hr, discharging, and sealing to obtain component B;
comparative example 3
The preparation was carried out in accordance with the composition and method of example 3, except that the carbon chain-extending silane coupling agent was not used.
The products obtained in examples 1 to 6 and comparative examples 1 to 3 were used to bond the article to be bonded to a bonding sheet and the data were measured.
1. Adhesion Strength and hardness test
The adhesive strength is implemented according to the GB/T7124 standard, and the specific test method comprises the steps of preparing a mixed colloid into a shear sample, and testing the adhesive strength, wherein the curing time is more than or equal to 3.5 hours; after soaking in water at 25 ℃ for 24 hours, testing the bonding strength; the hardness test was carried out according to the GB/T531.1 standard.
2. Water resistance test
Smearing the mixed colloid on the bonding material, wherein the curing time is more than or equal to 3.5 hours, the colloid thickness is controlled to be about 0.5mm, cutting the cured adhesive layer into sample strips with the width of 0.1mm at intervals, spraying the sample strips with liquid water at 25 ℃ for 24 hours, and recording the degumming percentage of the adhesive layer at different spraying times;
3. degumming test
Cutting the cured adhesive layer into sample strips with the width of 0.1mm at intervals, soaking the sample strips in water with the temperature of 65-75 ℃, and obtaining the stripping time of the adhesive layer and the time required for complete degumming;
TABLE 1
And (4) conclusion: the data in table 1 show that by matching a high functionality epoxy resin with a general bisphenol a type epoxy resin, the cured crosslink density is increased, thereby increasing the hardness and adhesion, which can be concluded from comparative example 1; the conclusion can be drawn through comparative examples 2 and 3 that comparative examples 2 and 3 show that the shear strength is low in a normal state, and comparative example 2 shows that the adhesive force is reduced greatly after the system is soaked in water for 24 hours; compared with the prior art, the degumming proportion of the modified polymer thiol is obviously excessive after being sprayed for 24 hours, because the modified polymer thiol has certain hydrophobicity, the introduced long carbon chain silane structure also has certain hydrophobicity, and the examples 5 and 6 are not degummed completely after being sprayed for 24 hours, so the bonding characteristic and the water resistance of the modified polymer thiol are superior to those of the prior art; the degumming performance of the example is almost the same as that of the comparative example, because the IPTS coupling agent of the system only reacts off a part of hydrolyzable groups in a polymercaptan system, and the degumming performance is also realized while the water resistance is ensured; on the basis of the prior art, the degumming performance of the water-resistant and degumming composite material is kept, the hydrophobic modification is carried out on the system, and the water resistance and the degumming performance are controlled to be in a state of a relative balance level.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be defined by the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (9)
1. The epoxy resin for cutting the water-resistant silicon rod comprises a component A and a component B, and is characterized in that: the component A uses bisphenol A epoxy resin as a matrix and uses high-functionality epoxy resin in a matching way, the component B comprises modified polymeric mercaptan and a long-carbon-chain silane coupling agent, and the long-carbon-chain silane coupling agent is at least one of the following structures;
wherein n is more than or equal to 7; r 1 ,R 2 ,R 3 Is methyl or ethyl;
the average functionality of the high-functionality epoxy resin is more than or equal to 3; the modified polymercaptan is obtained by modifying a polythiol curing agent by using isocyanatopropyl triethoxysilane or isocyanatopropyl trimethoxysilane as a modifying agent, wherein the weight ratio of the modifying agent to the polythiol curing agent is 0.1-5: 100.
2. the water-resistant epoxy resin for cutting silicon rods as claimed in claim 1, wherein the polythiol curing agent has an active hydrogen equivalent of 150 to 240, and the modifying method of the modified polythiol comprises the following steps: and (3) mixing the modifier with a polythiol curing agent, and fully reacting in a vacuum or nitrogen environment at the temperature of 25-35 ℃.
3. The water-resistant epoxy resin for cutting silicon rods according to claim 2, wherein: the component A and the component B comprise the following substances in parts by weight:
the component A comprises:
45 to 65 parts of bisphenol A epoxy resin
1 to 6 portions of high functionality epoxy resin
30 to 45 portions of filler
0.1 to 0.5 part of flexibilizer
0.01 to 2 portions of anti-settling agent
0.01 to 1 portion of defoaming agent
And the component B comprises:
30 to 60 parts of modified polymeric mercaptan
0.05 to 2 portions of long carbon chain silane coupling agent
0.05 to 1 portion of fatty amine
1 to 5 parts of accelerator
20 to 35 parts of filler
0.01 to 2 portions of defoaming agent
0.01 to 1 part of anti-settling agent.
4. The water-resistant epoxy resin for cutting silicon rods as claimed in claim 3, wherein: the bisphenol A type epoxy resin is at least one of E-20, E-44, E-51, E-54 or E-56; the high-functionality epoxy resin is at least one of F-51, F-44, F-50 and F-48.
5. The water-resistant epoxy resin for cutting silicon rods as claimed in claim 3, wherein: the toughening agent is an active diluent containing a monofunctional group or a difunctional group epoxy group, and the toughening agent is at least one of 1, 4-butanediol diglycidyl ether, 1, 6-hexanediol diglycidyl ether or dodecaglycidyl ether.
6. The water-resistant epoxy resin for cutting silicon rods as claimed in claim 3, wherein: the accelerant is at least one of triethylamine, 2,4, 6-tris (dimethylaminomethyl) phenol, pyridine, resorcinol, m-cresol or phenol; the amine value of the fatty amine is more than or equal to 500mgKOH/g.
7. The water-resistant epoxy resin for cutting silicon rods according to claim 3, wherein: the filler is at least one of calcium carbonate, silicon micropowder, talcum powder, aluminum oxide, aluminum hydroxide or silicon dioxide.
8. The water-resistant epoxy resin for cutting silicon rods according to claim 3, wherein: the anti-settling agent is at least one of fumed silica, organic bentonite or hydrogenated castor oil.
9. The method for preparing the epoxy resin for cutting the water-resistant silicon rod according to any one of claims 3 to 8, wherein the method comprises the following steps: the method comprises the following steps:
(1) Preparation of a component A: according to the material composition of the component A, according to the weight ratio, adding bisphenol A type epoxy resin, high functionality epoxy resin, a toughening agent, a filler, an anti-settling agent and a defoaming agent into a planetary stirrer, dispersing and mixing uniformly under a vacuum condition, and then discharging to obtain the component A;
(2) B, preparation of a component: according to the weight ratio of the material composition of the component B, stirring and dispersing the modified polymeric mercaptan and the long carbon chain coupling agent for 30 minutes at normal temperature under the closed condition of 55 percent RH, sequentially adding fatty amine, an accelerator, a filler, a defoaming agent and an anti-settling agent into dispersing equipment, and dispersing and mixing uniformly under the vacuum condition to obtain the component B;
(3) Mixing: the component A and the component B are mixed according to the weight ratio of A: b =1: and (3) uniformly mixing 0.8 to 2 to obtain the epoxy resin for cutting the water-resistant silicon rod.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011501984.3A CN112625218B (en) | 2020-12-17 | 2020-12-17 | Epoxy resin for cutting water-resistant silicon rod and preparation method thereof |
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